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Applications

Applications

A Novel Approach to Cleaning Validation for Pharmaceutical Manufacturing by Online SFE-SFC

Cleaning validation is necessary to establish the quality and safety of pharmaceutical drug products. The use of HPLC has increased due to the growing need for the individual analysis of products. However, manual sample prep processes may affect the quality of results. This paper evaluates the application of a novel on-line supercritical fluid extraction/chromatography system for cleaning validation.

 

Method Equivalency for The Analysis of Paracetamol

This application note proves equivalency of the Agilent 1260 Infinity LC and the Agilent 1260 Infinity II LC for the analysis of paracetamol and its impurities.

 

Separation of Statistic MMA-MAA Copolymers using Gradient SEC

Statistic copolymers of methyl methacrylate (MMA) and methacrylic acid (MAA) are widely used in pharmaceutical applications. Besides the molar mass distribution the chemical composition and the amount of comonomers in the copolymer is of importance. SEC-gradients is the method of choice to characterize these samples.

 

Big Pain Assays Aren't a Big Pain with the Raptor Biphenyl LC Column

The use of pain management drugs is steadily increasing. Therapeutic drug monitoring can be challenging due to the low cutoff levels, potential matrix interferences, and isobaric drug compounds.

 

Analyse Carbamate Pesticides in a Fraction of the Time and Boost Productivity

Carbamate pesticides are widely used insecticides that pose human and environmental health risks due to their activity as endocrine disruptors. While many pesticides can be analysed successfully using GC, carbamate pesticides are thermally unstable and degrade quickly in the hot GC inlet. Therefore, LC methods must be used to monitor levels of these semivolatile compounds in soil and water samples. C18 columns can be used for carbamate pesticides analysis, but traditional methods—such as EPA Method 531—require analysis times of over 20 minutes.
Using an Ultra Carbamate column instead of a C18 is a much better approach as this column was developed specifically for carbamates and allows much faster analysis times.

 

Rapid Detection of Chemicals Emitted from Museum Display Cases

This application note discusses assessment of volatile organic compounds emitted from the materials used in the manufacture of museum display cases, which can have a detrimental impact upon the condition of the artefacts within them. The note describes how sampling devices, such as Markes’ Micro-Chamber/Thermal Extractor, used in conjunction with analysis by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS) can allow rapid and convenient sampling of such chemicals from the wide range of construction materials used in these cases, and how new test schemes are being used by industry to certify these materials.

 

Determination of Iodinated Contrast Media in Aqueous Samples Using LC/MS/MS

Determination of iodinated contrast media in aqueous samples was performed by fast chromatography on an Agilent 1290 Infinity II LC coupled to an Agilent 6495 Triple Quadrupole LC/MS.

 

Extraction of Opiates from Whole Blood Using ISOLUTE® SLE+ Prior to GC/MS Analysis

This application note describes the extraction of opiate compounds from whole blood, prior to GC/MS analysis. This protocol also allows the simultaneous extraction of various other drugs of abuse classes: amphetamines, barbiturates, benzodiazepines and cocaine.

 

A Novel 75 cm Column Size Gives Increased Resolution and Better Sequence Coverage

The separation of complex peptide mixtures and their subsequent identification is crucial in the field of bottom-up proteomics. The increased peak capacity of the 75 cm column leads to enhanced quality of the separation, even when using similar gradients. Using even longer gradients can further improves results.

 

Online 2D-LC Characterization of Monoclonal Antibodies with Size Exclusion and Weak Cation Exchange

This application note demonstrates the combination of aggregation and charge variant analysis of monoclonal antibodies using the Agilent 1290 Infinity II 2D-LC solution.

 

Flavour Profiling of Premium Teas using HiSorb Sorptive Extraction and TD–GC–MS

This study compares the flavour profiles of three premium teas, obtained by high-capacity sorptive extraction using PDMS probes, with analysis by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS). The ability of the system to sample analytes from a range of chemical classes and volatilities is demonstrated.

 

Flavour Profiling of Alcoholic Spirits using HiSorb Sorptive Extraction and TD–GC–MS

This study shows that volatile and semi-volatile organic compounds (VOCs and SVOCs) at high and low levels in whisky and gin can be identified by high-capacity sorptive extraction using PDMS probes, with analysis by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS).

 

Flavour Profiling of Herbal Infusions using HiSorb Sorptive Extraction and TD–GC–MS

This study compares the flavour profiles of five herbal infusions, obtained by high-capacity sorptive extraction using PDMS probes, with analysis by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS). The ability of the system to sample analytes from a range of chemical classes and volatilities is demonstrated.

 

Flavour Profiling of Filter Coffee using HiSorb Sorptive Extraction and TD–GC–MS

This study shows that the wide range of volatile and semi-volatile organic compounds (VOCs and SVOCs) giving rise to the flavour of coffee can be identified by high-capacity sorptive extraction using PDMS probes, with analysis by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS).

 

Flavour Profiling of Milk using HiSorb Sorptive Extraction and TD–GC–MS

This study shows that the wide range of volatile and semi-volatile organic compounds (VOCs and SVOCs) giving rise to the flavour of milk can be identified by high-capacity sorptive extraction using PDMS probes, with analysis by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS).

 

Acid Herbicides in Water with On-line SPE-LC-MS/MS

This application note describes the use of ISOLUTE® ENV+ on-line cartridges in a fully automated on-line SPE-LC-MS/MS method for extraction and quantification of 16 acid herbicides in drinking and surface water.

 

Fast Routine Analysis of Polar Pesticides in Foods by Suppressed Ion Chromatography and Mass Spectrometry

This validated method enables the quantification of ten polar ionic compounds or four ionic pesticides and their metabolites in different food matrices by coupling ion chromatography to a triple quadrupole mass spectrometer.

 

Extraction of Illicit Drugs and Pesticides from Liver Tissue Using ISOLUTE® SLE+ Prior to GC/MS Analysis

This application note describes the extraction of a broad range of analytes from liver tissue matrix prior to GC/MS analysis using ISOLUTE® SLE+ supported liquid extraction columns. A protocol has been developed that allows the simultaneous extraction of various drugs of abuse classes: amphetamines, barbiturates, benzodiazepines, cocaine, ketamine, THC. In addition to these drug panels, simultaneous extraction of carbamate, organochlorine, organophosphate, pyrethroid, and triazine pesticide classes is demonstrated.

 

Routine, High-performance Analysis of Petrochemicals by GC×GC with Simultaneous Detection by FID and Tandem Ionisation TOF MS

This application note demonstrates the repeatability of a flow-modulated GC×GC–TOF MS system for the analysis of complex petrochemicals. The analytical approach described pushes the boundaries of hyphenated systems by simultaneously providing three information-rich datasets for each acquisition – namely, robust quantitation by FID, untargeted screening by TOF MS with electron ionisation (EI) at 70 eV, and confirmatory identification by TOF MS with soft EI.

 

Analysis of Synthetic Opiates and Novel Analgesics in Urine using SPE and HPLCMS/MS

Presented is a rapid, three step SPE procedure for the identification and quantification of fentanyl and its major urinary metabolite norfentanyl, in addition to four “designer” compounds: U-47700, W-18, W-15 and furanyl fentanyl. Due to the rapid use and abuse of fentanyl in medical and recreational settings, respectively, it is important to develop a method that would accurately extract this Schedule II drug from any other novel compounds that may be present.

 

Online 2D-LC Characterization of Monoclonal Antibodies Using Protein A and Weak Cation Exchange Chromatography

Protein A titer analysis and weak cation exchange chromatography for charge variant analysis were combined using the Agilent 1290 Infinity 2D-LC solution for the analysis of mAbs.

 

Simultaneous Extraction of Catecholamines and Metanephrines from Plasma for Analysis using LC-MS/MS

A highly sensitive, linear and rugged extraction procedure for catecholamines and metanephrines from human plasma is presented. Extraction was performed using EVOLUTE® EXPRESS WCX 10 mg 96-well plates and was shown to give good recoveries and precision with the quick Load-Wash-Elute protocol.

 

Time Saving, High Resolution GPC/SEC using Micro Columns and Optimized RI Detection

Efficient and fast separation for low molar mass polymers and proteins can be achieved using a combination of micro columns packed with smaller particles and optimized detectors. Although traditional analytical RI detectors, such as the SECcurity RI, profit from the higher resolution of micro columns, less peak broadening and higher resolution are the benefits that dedicated micro cell detection units offer.

 

Determination of 17 Mycotoxins in Cereals and Cereal Based Food Using Liquid Chromatography–Triple Quadrupole Mass Spectrometry

A simple and fast multi-mycotoxin method that covers the legislated mycotoxins as well as 3- and 15-acetyl-deoxynivalenol, deoxynivalenol-3-glucoside, nivalenol, its acetyl derivative fusarenon X and sterigmatocystin.

 

Proof of Long-Term, Leak-Free Performance for a Novel Self-tightening GC Column Nut

This application note demonstrates leak-free performance of a self-tightening (ST) column nut design that continually maintains pressure on graphite/polyimide ferrules over hundreds of injections.

 

Qualification of Headspace High Performance Septa by Headspace GC/MS

Headspace (HS) coupled with gas chromatography (GC) provides quantitative and qualitative information about the volatile components that are present in complex sample matrices. The Agilent 7697A Headspace Sampler is part of Agilent's line of gas chromatography products. Together with the market-leading 7890A GC, it has been demonstrated to provide industry leading performance.

 

Evaluation of the Ultra Inert Liner Deactivation for Active Compounds Analysis by GC

Endrin and DDT breakdown and active semivolatiles tests were used for the Ultra Inert liner deactivation performance evaluation. The results indicate that the Ultra Inert deactivated liners provide superior inertness for analysis of active compounds.

 

Analysis of Residual Chloramphenicol in Shrimp by LC/MS/MS with QuEChERS Sample Pre-treatment

Chloramphenicol (CAP) is a broad spectrum antibiotic that is widely used in the growth of animals and marine culture. However, CAP can cause aplastic anaemia and is a possible carcinogen in humans. Its use in livestock farming including fish and shrimps has been banned in the European Union and many other countries. Here, we present an LC/MS/MS method for accurate and reliable quantitation of CAP in shrimp samples on an LCMS-8050 with a heated ESI interface.

 

Multi-Component Analysis of Five Beers

In this application note, we describe the simultaneous analysis of five commercially available beers with a triple quadrupole mass spectrometer (LCMS-8060 ) using a primary metabolite method package, and performing principal component analysis on the data set obtained using TraverseTM MS software. 

 

Analysis of Glufosinate, Glyphosate, and AMPA in Drinking Water Using a Triple Quadrupole LC/MS/MS System

Glufosinate is a popular amino acid-based herbicide and glyphosate a popular foliage treatment herbicide. Glyphosate metabolizes in soil or water to form aminomethylphosphonic acid (AMPA). In this example, Appendix Method 22 is used to analyze glufosinate, glyphosate, and AMPA. In addition, by using the LCMS-8050, samples can be analyzed directly without the pretreatment process of concentrating samples by solid phase extraction.

 

Multi-component Quantitative Analysis of Pharmaceuticals in the Environment by UHPLC-MS/MS with On-line SPE

Many common drugs can be found in the environment and sometimes even in drinking water. These drugs and their metabolites get into the waste water through excretion via the urine or feces and may reach surface water, groundwater and also drinking water after the passage in the sewage treatment plants. This study describes a novel multi-residue UHPLC-MS/MS method that utilizes an online SPE enrichment of the various compounds followed by a fast and optimized chromatographic gradient.

 

Using the Nexera UC Online SFE-SFC-MS System to Analyze Residual Pesticides in Agricultural Products

The Nexera UC online SFE-SFC-MS system combines supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) in one online system, so that the entire process from extraction of target components to acquisition of data can be performed completely automatically. This article describes an example of using the Nexera UC online SFE-SFC-MS system to analyze residual pesticides in agricultural products.

 

Direct Determination of Trace Hormones in Drinking Water by Large Volume Injection using the LCMS-8050 Triple Quadrupole Mass Spectrometer

Endocrine disrupting compounds enter the aquatic environment primarily through the discharge of treated and raw sewage and are detrimental to aquatic organisms even at subnanogram per litre levels. In this study, the LCMS-8050 triple quadrupole mass spectrometer was used for the highly selective and sensitive detection of hormones in water to meet the requirements of UCMR3.

 

Simultaneous Analysis of 16 Sweeteners Using Triple Quadrupole LC/MS/MS [LCMS-8050]

Artificial sweeteners such as aspartame, sucralose, and acesulfame potassium fall under the category of designated additives according to Japan's Food Sanitation Act, and prescribed standards are in place for their use in some foods and quantities. In this application note, an example of the simultaneous analysis of 16 sweeteners using an LCMS-8050 is presented.

 

Analysis of Dioxins in Feed and Food Using GC-MS/MS as Confirmatory Method in Complying with EU Regulation

Polychlorinated dibenzodioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) are generally termed as dioxins. It has been reported that dioxins accumulate in the environment, plants and organisms due to their good chemical stability and good solubility in animal fats. In this study, Shimadzu’s GCMS-TQ8040, a new model GC-MS/MS, was employed and evaluated for identification and quantification of the seventeen most toxic PCDD and PCDF congeners listed by the EU regulation.

 

UHPLC-MS Analysis of Glycosylation

The characterization of glycan pattern is a major quality parameter in the production of biotherapeutics. TSKgel Amide-80 2 μm was used for glycosylation analysis of labelled glycans of various antibody samples by both fluorescence detection and mass spectrometric detection.

 

Analysis of HMWS of Antibodies and Metalloproteins

This application note demonstrates the superior resolving power of the TSKgel UltraSW Aggregate column for the analysis of high molecular weight species (HMWS) of monoclonal antibodies and metalloproteins formed under forced denatured conditions, including acid and thermal denaturation.

 

DAR Analysis of Antibody Drug Conjugates (ADC)

Antibody-drug conjugates (ADCs) represent some of the most promising antibody drug candidates for next-generation biopharmaceuticals. Hydrophobic interaction chromatography can be applied to determine the drug-to-antibody ratio (DAR) of an ADC. In this application note an ADC was analysed using a TSKgel Butyl-NPR column.

 

Determination of mAb Charge Heterogeneity

Charge isoforms of proteins result from deamidation or from incomplete removal of the C-terminal lysine residue. Ion exchange chromatography is the method of choice to analyse charge heterogeneity of proteins. TSKgel STAT series columns provide a high resolution of isoforms in short analysis time and are ideally suited for the QC of biotherapeutics by UHPLC or HPLC.

 

UHPLC Aggregate Analysis

Analytical size exclusion chromatography (SEC) is widely used to determine the ratio of aggregates, dimers, monomers, and fragments in monoclonal antibody (mAb) formulations. This application describes the use of a TSKgel UP-SW3000 SEC column for fast and accurate mAb aggregate analysis without compromising the quality of the aggregate determination or reproducibility.

 

Fast mAb Titer Determination by HPLC

Antibody titer determination in cell culture supernatants by Protein A affinity HPLC is much more robust, reliable and reproducible than enzyme-linked immunosorbent assays (ELISAs). The quick capture and accurate titer analysis over a wide concentration range is demonstrated using a TSKgel Protein A-5PW column.

 

Optimizing Extraction of Multianalyte Suites from Water Samples Using Layered Solid Phase Extraction Columns

This innovative SPE technique is used in applications where multiple suites of analytes with a broad polarity range are to be extracted simultaneously from a single water sample, such as organochlorine, triazine and organophosphate pesticides, or endocrine disrupters.

 

Analysis of Pharmaceuticals in Water Using Automated On-line SPE-LC-MS/MS

This application note describes the use of EVOLUTE® EXPRESS ABN on-line cartridges for extraction of 13 commonly prescribed pharmaceuticals in water. This is an automated on-line SPE-LC-MS/MS method where the SPE is fully integrated into the analytical workflow.

 

Advice on Sorbent Selection, Tube Conditioning, Tube Storage and Air Sampling

Selection of the correct sorbent or series of sorbents for sampling and release of the analytes of interest is one of the most important factors when developing a valid and robust thermal desorption method. This application note gives advice on which sorbent to use for pumped or diffusive tube monitoring of various vapour-phase organics, and suggests parameters for conditioning and storing packed tubes.

 

Equivalency for The Analysis of Tricyclic Antidepressant Drugs

This application note proves equivalency of the Agilent 1200 Series LC and the Agilent 1260 Infinity II LC for the analysis of tricyclic antidepressant drugs.

 

Evaluating the Performance of the OneNeb Series 2 Nebulizer with PerkinElmer Optima 7/8x00 Series ICP-OES Systems

This application note demonstrates the superior performance of the OneNeb Series 2, with up to four times greater sensitivity, improved detection limits, and improved reproducibility, especially with challenging samples such as those with high levels of dissolved solids.

 

Use of the Agilent Multimode Sample Introduction System (MSIS) for Simultaneous Hydride Determination and Conventional Nebulization Using the PerkinElmer Optima 7/8x00 Series ICP-OES Systems

Vapour generation techniques are routinely used with ICP-OES and AAS for the determination of trace levels of environmentally sensitive elements including arsenic (As), selenium (Se), and other elements using the hydride generation technique, plus mercury (Hg) using the cold vapour technique. Determination using hydride generation or cold vapour techniques has advantages including improved sensitivity, simplicity, and reduced interferences, as volatile hydrides are separated from the sample matrix. This application note outlines a method for performing simultaneous hydride determination and conventional nebulization.

 

Analysis of Nutrients, Minerals and Trace Elements in Drinking and Recycled Water Samples using the PerkinElmer AAnalyst 800 Atomic Absorption Spectrometer with Agilent Supplies

The World Health Organization has noted that there is a pressing need for comprehensive and accurate assessment of water quality. To address the consequences of contamination threats, accurate monitoring of minerals and contaminants in drinking, waste, surface, and ground waters is essential to ensure good water quality. In this study, municipal drinking water, recycled water, and bottled water samples were analysed for seven different elements using the Perkin Elmer AAnalyst 800 FAAS. 

 

Extraction of Estrone and Estradiol from Human Serum Using ISOLUTE® SLE+ Prior to HPLC-MS/MS

Estrone (E1) and estradiol (E2) are female steroid hormones typically monitored in peri- and postmenopausal human serum samples to assess a number of conditions. This application note describes a simple supported liquid extraction method for extraction of estrone and estradiol from human serum. An analytical HPLC-MS/MS method that avoids the use of derivatization or fluoride adduct stabilization (two approaches often used to enhance method sensitivity) is used. High, reproducible analyte recovery and low detection limits are achieved.

 

Multiclass Veterinary Antibiotics on Raptor™ C18 by LC-MS/MS

To regulate the proper use of veterinary antibiotics, the US FDA has set maximum residue limits (MRL) for a variety of animal tissue and food products (21 CFR Part 556). A sensitive, efficient, and reliable analytical method for different classes of antibiotics is necessary to meet this regulation, and the Raptor™ C18 LC column is reportedly the ideal choice.

 

Fast and Confident Quantitation of Environmental Contaminants using GC–TOF MS

This application note demonstrates how the excellent sensitivity, stability and high-quality spectra produced by BenchTOF mass spectrometers, with data analysis by TOF-DS software, can provide a rapid and robust solution for the quantitative analysis of environmental contaminants.

 

Screening Method for Fluoroquinolones Using an Advanced UHPLC Column and System Combination

Fluoroquinolones are popular broad spectrum antibiotics used in animal husbandry, some of which have been banned by US FDA and EU regulations. This application demonstrates the advantages of using the Thermo Scientific™ Hypersil GOLD™ VANQUISH™ 1.9 μm UHPLC column, in conjunction with the Vanquish UHPLC system and Chromeleon software to screen for fluoroquinolones. This combination offers excellent peak resolution, outstanding retention time reproducibility and consistent data processing.

 

Fast Screening and Quantification of Pesticide Residues Using a Comprehensive LC-MS Solution: The Pesticide Explorer Collection – Standard Quantitation

The Thermo Scientific™ Pesticide Explorer Collection is a comprehensive set of LC-MS solutions designed for laboratories performing routine quantitation, targeted and non-targeted screening of pesticide residues in food matrices.

 

Equivalency for The Analysis of Antihistaminic Drugs

This application note proves equivalency of the Agilent 1100 Series Quaternary LC and the Agilent 1260 Infinity II LC for the analysis of antihistaminic drugs.

 

Rapid Profiling of VOCs and SVOCs in e-cigarette Vapours for Regulatory Compliance and Quality Control

This application note describes a simple, quick TD-based approach for the sampling and analysis of target compounds (such as nicotine, impurities and flavour compounds) in vapours from flavoured e-cigarettes. Used in conjunction with GC–MS analysis, the result is a versatile screening method for tackling the challenge of regulatory compliance and quality control in this rapidly expanding industry.

 

Bio-SPME(固相マイクロ抽出)を用いた微量サンプリング法の開発と乾燥血液スポット(DBS)との比較

本研究では、生体試料マトリックスに対してHPLC、UHPLC およびLC/MS 分析に先立って行うことのできる微量サンプリング法として、固相マイクロ抽出(SPME)を紹介します。

 

Simultaneous Determination of Prescription and Designer Benzodiazepines in Urine by SPE and LC-MS/MS

Benzodiazepines, frequently referred to as “Benzos”, are prescribed for the treatment of anxiety, insomnia, muscle spasms, alcohol withdrawal and seizure-prevention on account of their ability to depress the central nervous system. Similar to other commonly abused compounds, such as cannabinoids or amphetamines, “legal” alternatives have been developed for Benzos as well in an attempt to bypass the controlled substances act. These new designer drugs are structural or functional analogs of the controlled substance designed to not only mimic the pharmacological effects of the original drug, but also avoid illegal classification and/or detection in a standard drug test. Given that these compounds are derived from “template structures”, it will prove valuable for labs to have a method that can not only target current metabolites of interest, but also the latest ones being formulated.

 

Thyroid Hormones in Serum and Plasma Using SPE Extraction and UHPLC-MS/MS Analysis

Thyroid hormones are endogenous hormones that play an important role in many biological processes, including growth, development and metabolism. Most of the thyroid hormones circulating in the blood are bound to proteins and only a small fraction of circulating hormones are in their biologically active free form (unbound). This application note describes the development of an analytical method for the sensitive and accurate determination of free and total thyroid hormones in serum and plasma using a mixed-mode SPE extraction procedure and UHPLC-MS/MS analysis. Chromatographic separation, including baseline resolution of triiodothyronine and reverse triiodothyronine, is conducted in 3 minutes using a Selectra® DA column. 

 

Determination of 11-nor-9-Carboxy-THC in Human Urine by QuEChERS and LC-MS/MS

11-nor-9-Carboxy-THC, also known as THCA or carboxy-THC, is the main secondary metabolite of THC (the active component of marijuana) formed in the human body. THCA is excreted in urine in the form of glucuronide conjugates. Typical sample preparation methods for THCA in urine include liquid-liquid extraction (LLE) and solid phase extraction (SPE). This application utilizes a novel sample preparation technique, QuEChERS to effectively quantitate THCA levels in human urine.

 

Detection of Aflatoxins in Milk at Picogram Levels Using SPE and LC-MS/MS

Aflatoxins are naturally occurring mycotoxins that are produced by several species of fungi (Aspergillus flavus and Aspergillus parasiticus).  They are classified by the International Agency for Research on Cancer as group 1 carcinogens (compounds known to be carcinogenic in humans). Aflatoxins can occur in milk as a result of dairy animals consuming contaminated feed. This application note outlines a method for the low level determination of aflatoxins in milk using a polymeric solid-phase extraction (SPE) cartridge. Analysis is performed by LC-MS/MS using a Selectra® DA HPLC column. The method was optimized to allow the detection of aflatoxins at the low regulatory concentrations required. 

 

Determination of Patulin in Processed Foods Using QuEChERS Extraction and UHPLC-MS/MS Analysis

Patulin is a naturally occurring mycotoxin that is produced by several species of fungi, such as Aspergillus, Penicillium and Byssochlamys. It typically grows on fruit, including apples, pears, peaches and grapes, but has also been reported in vegetables and cereal grains. This application note outlines a QuEChERS procedure for the detection of patulin in processed food products. Analysis is carried out by UHPLC-MS/MS using a Selectra® DA column. The unique chemistry of the Selectra® DA column, which contains a polyaromatic stationary phase, provides a high degree of retention and selectivity for aromatic compounds and improved retention of polar compounds.

 

EPA Method 1694: Analysis of Pharmaceuticals and Personal Care Products in Water

EPA Method 1694 was published in December 2007 as a screening method for the analysis of pharmaceuticals and personal care products (PPCPs) in environmental samples, including water (wastewater, surface water and drinking water). The PPCPs include common prescription drugs, veterinary drugs, over‐the‐counter medicines, dietary supplements and other consumer products. This application note outlines a SPE procedure using UCT’s Enviro-Clean® HL DVB polymeric sorbent and Selectra® DA HPLC column for the determination of 64 PPCPs in water according to EPA Method 1694.

 

Extraction of Synthetic and Naturally Occurring Cannabinoids in Urine Using SPE and LC-MS/MS

Synthetic cannabinoids (Spice) are a family of compounds that when consumed mimic the effects of marijuana. The biggest hurdle for testing facilities is keeping up with the ever-changing synthetic analogs being produced by illicit drug makers in an attempt to avoid detection. 

 

Comprehensive Insights into Tobacco Smoke Constituents using TD–GC×GC–TOF MS with Tandem Ionisation

This Application Note demonstrates the enhanced separation and unparalleled sensitivity that can be achieved in the characterisation of cigarette smoke, using thermal desorption (TD) and GC×GC with BenchTOF time-of-flight mass spectrometry, aided by Tandem Ionisation for simultaneous acquisition of hard and soft EI data.

 

Determination of Sweeteners, Preservatives, and Caffeine in Food

Analysis of additives such as sweeteners, preservatives, and caffeine in various food products, beverages, and consumer toothpaste using the Agilent 1290 Infinity II LC. 

 

GC Analysis of Glycols in Toothpaste Using Agilent J&W DB-Wax Ultra Inert Capillary GC Columns

This application note demonstrates the excellent inertness performance of an Agilent J&W DB-Wax Ultra Inert GC column in the analysis of glycols in toothpaste. DB-Wax UI columns provide better column durability and more consistent analytical results compared with other PEG stationary phase GC columns.

 

Analysis of Distilled Spirits Using an Agilent J&W DB-WAX Ultra Inert Capillary GC Column

The Agilent J&W DB-WAX Ultra Inert GC column has excellent stability for distilled spirit samples containing high levels of water or water-ethanol mixture. The high inertness performance of the column ensures good peak shapes for problematic volatile congeners including alcohols, aldehydes, and organic acids.

 

Lavender Oil Analysis Using Agilent J&W DB-WAX Ultra Inert Capillary GC Columns

Lavender essential oil samples were analyzed using the Agilent J&W DB-Wax Ultra Inert GC column and DB-Wax GC column by GC/FID and GC/MSD. Thirty-six major components were identified. The DB-Wax Ultra Inert GC column showed the same selectivity as the DB-Wax GC column. The DB-Wax Ultra Inert GC column however, generated better peak shape and improved sensitivity for active compounds for complex essential oil analysis.

 

多機能カラムSupel™ Tox を使用した乳中のアフラトキシンM1 のLC/MS 分析

他のSPE 法でみられる手順が多く煩雑な前処理(保持・溶出)とは異なり、Supel(スペル) Tox(トックス) AflaZea(アフラゼア) では「妨害物除去」 操作を用い、洗浄ステップを無くして時間を短縮した。

 

血漿中ステロイドホルモンのLC/MS/MS分析における前処理法の開発

HybridSPE(ハイブリッドエスピーイー)®-Phospholipid(ホスホリピッド) 96穴プレートを前処理に使用した血漿中ステロイドホルモンの分析例を紹介する。定量に影響するリン脂質を除去する事によって優れた回収率を得ると同時に、カラム寿命を延長させる事が実現した。

 

Ascentis Express UHPLCコアシェルカラム ・粒子径2.0 μmのFused-Core

Supelco(スペルコ) Ascentis(アセンティス)® Express(エクスプレス)カラムシリーズは2.0 μmのFused(フューズド)-Core(コア)シリカ粒子を使用し、UHPLC装置における分離性能を最大限に引き出す事が可能になる。

 

EP/USP GPC/SEC Molar Mass Determination for Low Molecular Weight Heparin (LMWH)

LMWHs are defined as heparin salts having an average molecular weight of less than 8000 Da. Both, the Pharmaeuropa and the US Pharmacopeia, require GPC/SEC to characterize e.g. Enoxaparin Sodium or other low molar mass heparins with respect to molecular weight. A dedicated GPC/SEC software such as PSS WinGPC UniChrom is required to obtain reliable mass fraction information.

 

Analysis of Polycyclic Aromatic Hydrocarbons by 2D-LC

PAHs were determined in a petroleum vacuum distillation residue using the Agilent 1290 Infinity Multiple Heart-Cutting 2D-LC solution with normal-phase in the first dimension and reversed-phase in the second dimension.

 

Comprehensive Guide to Applications of Time-of-Flight Mass Spectrometry

This new 40-page guide describes 30 examples of applications that benefit from TOF MS, ranging from cheese aroma profiling to crude oil fingerprinting using GC×GC and much more besides. With concise descriptions of key analytical challenges, and clear diagrams showing how TOF MS technologies can help address them, this guide is a valuable source of information for every GC analyst.

 

EPA Method 544: Determination of Microcystins and Nodularin in Drinking Water by SPE and LC-MS/MS Detection

Microcystins are a group of hepatotoxins produced by freshwater cyanobacteria (also known as blue-green algae). Microcystins can be generated in large quantities during algae blooms and can pose a major risk to surface, ground and drinking water. This application note outlines a SPE method for the determination of 6 microcystins and nodularin in drinking water according to EPA Method 544. A 500 mL water sample is passed through a 6 mL UCT Enviro-Clean® SPE cartridge containing 150 mg of divinylbenzene (DVB) based sorbent to extract the analytes. The final purified extract is then analyzed by LC-MS/MS equipped with a Selectra® C8 HPLC column.

 

Increased Monoclonal Antibody Resolution with TSKgel® UP-SW3000 Columns

With the growing market for therapeutic antibodies, the demand for high performance analytics via liquid chromatography is increasing. Most important are the resolution over a wide range of molecular weights while reducing analysis times. The TSKgel UP-SW3000 series for SEC successfully addresses this challenge: its 2 µm particle size improves the resolution for antibody monomers, fragments and aggregates – all this in half the analysis time. 

 

Enhanced Productivity for The Analysis of Ore Samples

The Niagara Plus sample introduction accessory has greatly enhanced the performance of ICP-OES and ICP-MS instruments. The accessory uses Flow Injection technology to reduce analysis time by 50%, typically, resulting in reduced environmental impact and lower operating cost. This report highlights the performance of the Niagara Plus at the Marine and Freshwater Research Laboratory (MAFRL) at Murdoch University. The data discussed is from a  project examining ore samples for mineral processing. 

 

How to Achieve High Accuracy with Difficult Samples

It is very common for ICP labs to encounter samples with a varying degree of total dissolved solids (TDS). However samples with high TDS, 5 to 20%, can often pose many analytical challenges for the ICP analyst. These challenges include short torch lifetime and interrupted analyses due to a clogged nebulizer or injector. This report highlights a collaboration with Inorganic Ventures in which we describe how to optimize the sample introduction system and method parameters of the ICP to better handle high TDS samples. The performance achieved with a newly introduced fully ceramic D-Torch for the Spectro Arcos EOP (Axial) ICP-OES is also described.

 

Uninterrupted and Maintenance-Free ICP Operation

It is standard operation to use dry argon as your ICP nebulizer gas in order to generate an aerosol and transport the sample to the plasma. However, when dealing with samples containing high amounts of total dissolved solids (TDS) you have an increased likelihood of salt deposits forming at the tip of the nebulizer and injector; this can result in a failed analysis due to a drift in signal or an extinguished plasma. In order to handle a challenging sample matrix, such as high TDS, it is important that you optimize your ICP sample introduction system. Glass Expansion designed the new ElegraTM argon humidifier to provide an efficient, but simple to use humidifier for ICP-OES and ICP-MS applications. In this article we will focus on the advantages of the Elegra design and the benefits of adding a humidifier for high TDS applications. 

 

EPA Method 530: Determination of Selected Semivolatile Organic Chemicals in Drinking Water by SPE and GC/MS

Recently the US EPA published a list of 30 UCMR4 (the 4th Unregulated Contaminant Monitoring Rule) analytes, which may potentially be present in tap water but are not yet subject to EPA’s drinking water standards set under the Safety Drinking Water Act. Four among the 30 UCMR4 compounds, including o-toluidine, quinoline, butylated hydroxyanisole (BHA), and dimethipin, are determined by EPA method 530 using solid phase extraction (SPE) and GC/MS detection. In this study, analytes were extracted using UCT’s divinylbenzene based sorbent (HLDVB). A GC/MS SIM method with solvent standard calibration was carried out for data acquisition and analyte quantitation.

 

HPLC to UHPLC Transfer of USP Method for Amlodipine Besylate

This application note describes the method transfer of a USP HPLC method for amlodipine besylate tablets to a UHPLC method using the Agilent 1290 Infinity II LC.

 

Analytical Method for Polycyclic Aromatic Hydrocarbons (PAHs) in Yerba Mate Tea Using Modified QuEChERS, Solid Phase Extraction and GC-TOFMS and GC-MS/MS

Polycyclic aromatic hydrocarbons (PAHs) are toxic compounds found in some foods, especially those that are smoked, roasted, grilled, or dried during preparation. Yerba mate (Ilex paraguariensis ) tea is of particular interest because of relatively high PAH levels and proposed links between yerba mate tea and health problems.

 

Highly Sensitive Aroma-profiling of Cantaloupe Melon by TD–GC–TOF MS

The accompanying paper (reproduced here with the permission of the publishers) shows how a method based on grab-sampling, thermal desorption (TD), gas chromatography (GC) and time-of-flight mass spectrometry (TOF MS) can be used to elucidate the key volatiles from cantaloupe melon, and how these vary with size of the melon pieces. Specifically, it focuses on the sensitivity enhancement offered by the use of the TD-100™ thermal desorber and the BenchTOF-HD™ mass spectrometer, and highlights how such analytical information will be of value in efforts to improve food flavour, understand shelf life, and detect microbial contamination.

 

Comparison of The Aroma Profiles of Hops by TD–GC–TOF MS with Select-eV Variable-energy Electron Ionisation

This application note demonstrates the high performance of a TD–GC–TOF MS system for the analysis of complex aroma profiles from hops. The use of complementary soft electron ionisation provides enhanced confidence in the identification of terpenoids, while the comparison of hop varieties is simplified by near-real-time analysis in the accompanying software package.

 

Determination of Beta-Blockers in Urine Using SFC/MS

This application note demonstrates the separation and quantification of beta-blockers, listed as prohibited substances by the World Anti-Doping Agency, in urine using the Agilent 1260 Infinity Analytical SFC System.

 

Determination of Patulin in Apple Juice Using SPE and UHPLC-MS/MS Analysis

Patulin is a naturally occurring mycotoxin that is produced by several species of fungi, such as Aspergillus, Penicillium and Byssochlamys. It typically grows on fruit, including apples, pears, peaches and grapes, but has also been reported in vegetables and cereal grains. This application note outlines a simple solid-phase extraction (SPE) procedure for the low level detection of patulin in apple juice. Analysis is carried out by UHPLC-MS/MS using a Selectra® DA column. The unique chemistry of the Selectra® DA column, which contains a polyaromatic stationary phase, provides a high degree of retention and selectivity for aromatic compounds and improved retention of polar compounds.

 

Acidic, Basic, and Neutral Drug Screen of Hydrolyzed Urine Using Supported Liquid Extraction Prior to LC-MS/MS Analysis

Appropriate for urine screening purposes, this application note describes the extraction of acidic, basic, and neutral drugs using ISOLUTE® SLE+ supported liquid extraction plates. The limit of detection for the 32 drugs in the suite was determined and was found to range from 5 ng/mL to 1.25 ng/mL.

 

Gentamicin Sulfate with Pulsed Amperometric Detection

This application notes describes the determination of gentamicin sulfate applying pulsed amperometric detection after post-column addition of NaOH. Gentamicin consists of several closely related compounds, namely gentamicin C1, gentamicin C1a, and gentamicin C2, C2a and C2b. In spite of the structural similarity, IC achieves a good separation of the different gentamicin compounds.

 

Simple and Reliable Quantitation of ppt-level PAHs in Air by TD–GC–MS

This application note describes the performance of a sorbent tube and optimised analytical protocol dedicated to the detection of ppt-level polycyclic aromatic hydrocarbons (PAHs) in ambient air. Using active (pumped) sampling with analysis by thermal desorption–gas chromatography (TD–GC), this innovative approach completely avoids the labour-intensive solvent-extraction protocol employed in many standardised methods. 

 

Ultrafast Analysis of Food Preservatives

This application note demonstrates ultrafast gradients with an over 60% reduction of analysis time using the Agilent 1290 Infinity II Multisampler with dual-needle function and alternating column regeneration.

 

リンゴ中のパツリンにおける低濃度UHPLC分析

本試験の目的は、前処理カラムSupelMIP® SPE とUHPLC を用いてリンゴピューレ中に標準添加したパツリンを濃縮して分析することです。

 

SPME LC チップを用いた尿中乱用薬物におけるLC/MS分析

本報告では、尿サンプル中に存在する違法薬物代謝物の抽出にSPME を利用し、その後LC/MS/MS 分析を行う方法について示します。

 

尿中の薬物代謝物におけるUHPLC-TOF/MS分析

本試験の目標は、UHPLC/MS(TOF)の分析前に、さまざまな種に由来するβ- グルクロニダーゼで各化合物群を加水分解するための最適条件を決定することです。

 

UHPLC/MS/MSを用いた牛乳、粉ミルク中のvitamin D 分析

牛乳、乳製品をはじめ、乳児・大人用栄養食品へのvitamin D 強化が、vitamin D を補給するために多くの国で義務付けられています。

 

UHPLC カラム「TITAN C18」を用いたエストラジオールの非誘導体化LC/MS/MS 分析

LC/MS/MS 法は選択性が改善されることが認められているため、性ステロイドホルモン測定の選択肢になりつつあります。

 

Quantitative Analysis of Pesticides in QuEChERs Extracts Using APGC/MS/MS

The purpose of this note was to detect and quantify GC-amenable pesticides in QuEChERs extracts of fruit and vegetables and demonstrate the limits of detection and linearity possible using APGC/MS/MS.

 

Enhancing MRM Experiments in GC/MS/MS Using APGC

Gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) are the techniques of choice in pesticide residue analysis (PRA) for a wide variety of sample matrices. The aim of the project was to evaluate the potential of APGC–Xevo TQ-S for the quantitative analysis of pesticides in foodstuffs: 25 pesticides with varying chemical properties have been selected and the potential advantages of APGC were evaluated in comparison with EI ionization.

 

Minimizing Carryover During Dioxin Analysis Using the Xevo TQ-S with APGC

Dioxins and furans are produced when organic compounds are incinerated in the presence of chlorine for example during PVC production, paper bleaching, and from natural sources such as volcanoes. The purpose of this study was to eliminate carryover from sample to sample to ensure accurate quantification of unknown dioxin and furan containing samples.

 

Increasing the Abundance of Precursor Ions for Multiple Reaction Monitoring (MRM) Analysis by Atmospheric Pressure GC (APGC) Ionization

The goal of this note was to compare the ionization and fragmentation characteristics of pesticides using traditional electron ionization (EI+) GC-MS and APGC to improve MRM analysis of these compounds.

 

Detection of Unexpected Contaminants During Consumer Protection Analysis in Support of Restriction of Hazardous Substances (RoHS) Legislation

In this note, the aim is to demonstrate the advantages of collecting multiple reaction monitoring (MRM) and MS scan data in parallel (RADAR™ acquisition), in support of consumer protection legislation using Xevo® TQ-S MS System with an APGC Source.

 

A Validated Method for the Analysis of 142 Pesticide Residues Using Atmospheric Pressure GC Coupled with Tandem Quadrupole Mass Spectrometry

Pesticides are widely used in agricultural activity across the globe and residues of these pesticides in food products destined for human consumption can be a major food safety risk. Pesticide residues are high on the list of consumer concerns and consequently laboratories are tasked to screen samples for as many pesticides as possible in a single analysis within an appropriate timescale. In this application note we describe the development and validation of a multi-class method for the routine determination of 142 pesticide residues in various fruit and vegetable matrices.

 

Tube and Trap Impedance Testing on the TurboMatrix 650 ATD Thermal Desorber

For a thermal-desorption analysis to be successful, the adsorbent inside each tube and secondary trap must be properly packed. Any voids caused by settlement or contraction of the packing may induce channelling of the gas flow during pumped sampling and thermal desorption. Such effects may also disturb the geometry of the ‘air gap’ which is critical for predictable performance in diffusive sampling.

 

Ultra-sensitive Detection of Pharmaceutical and Personal Care Products in Water with an Integrated On-Line Extraction (OLE)-UHPLC-MS/MS System

An advanced ultra-high performance liquid chromatography (UHPLC) method was developed for the quantification of trace pharmaceutical and personal care products (PPCPs) in clean water. The Bruker Advance™ UHPLC system, with integrated on-line extraction (OLE) coupled to the EVOQ LC-MS/MS detected 1-2 ppt levels of PPCPs in water with a linear response up to 200 or 500 ppt. Excellent system robustness was obtained throughout the extended method development and sample analysis period.

 

Analysis of Volatile Organic Compounds (VOCs) in Air Using US EPA Method TO-17

Optimized methods are needed for the analysis of toxic compounds in air to understand the impact to human health. EPA Method TO-17 is used to determine toxic compounds in air after they have been collected onto sorbent tubes. This application note demonstrates that the PerkinElmer TurboMatrix™ Thermal Desorber and the PerkinElmer Clarus® SQ 8 GC/MS will meet and exceed the criteria set forth in EPA method TO-17. Detailed instrument method parameters are presented, with precision, recovery, linearity and detection limit results.

 

The Analysis of Common Drugs of Abuse in an Oral Fluid Matrix using A New Q TRAP® Platform

The multiplexing analysis of several compound classes, such as common prescription drugs along with drugs of abuse is very important. The measurement of these drugs has generally been performed using urine as the sample matrix. In the present study a fast, robust, and reliable method was developed for the detection of 15 compounds in an oral fluid matrix. The LC-MS/MS methods were performed using Multiple Reaction Monitoring (MRM) along with fast positive negative switching detecting all compounds with Limits of Quantitation (LOQ) in-line with the current recommended cutoffs. Throughput was also considered by using the MPX™-2 high throughput HPLC system where an increase in sample throughput of 142% was observed.

 

Targeted and Non-Targeted Screening for Drugs with High Confidence using the AB SCIEX TripleTOF™ 4600 System and Intuitive Data Processing Tools

The high resolution and accurate mass AB SCIEX TripleTOF™ 4600 LC/MS/MS system was used to screen for drugs from forensic equine urine, and to quantify drug compounds with excellent accuracy and high reproducibility. Fast Information Dependent Acquisition (IDA) MS/MS spectra were used to additionally confirm the identity of detected compounds based on mass spectral library searching. The acquired full scan MS and MS/MS data can further be used in a general unknown comparative screening workflow in which a sample-control comparison can be made for easy, fast and reliable identification of compounds present in the sample.

 

Targeted and Non-Targeted Screening for Drugs with High Confidence using the AB SCIEX TripleTOF™ 4600 System and Intuitive Data Processing Tools

The high resolution and accurate mass AB SCIEX TripleTOF™ 4600 LC/MS/MS system was used to screen for drugs from forensic equine urine, and to quantify drug compounds with excellent accuracy and high reproducibility. Fast Information Dependent Acquisition (IDA) MS/MS spectra were used to additionally confirm the identity of detected compounds based on mass spectral library searching. The acquired full scan MS and MS/MS data can further be used in a general unknown comparative screening workflow in which a sample-control comparison can be made for easy, fast and reliable identification of compounds present in the sample.

 

Advanced Automated Library Searching for Compound Identification in Forensic Toxicology Samples

LC-MS/MS utilization in forensic toxicology screening for drugs and drug metabolites has become increasingly popular due to the selectivity, sensitivity and the speed of LC-MS/MS analysis. MS/MS confirmation with automated searching against available spectral libraries has proven to add a superior level of confidence to the compound identification.

 

Evidence of Cathinones Use Through Hair Analysis using LC-MS/MS

During the last few years, there has been a rapid growth in the availability of new synthetic substances (commonly known as ‘legal highs’) in the UK and throughout Europe, the majority of which are freely available over the internet or in ‘head shops’. SCIEX has developed and validated a novel method for a range of cathinones in hair by LC-MS/MS to include: cathinone, methcathinone, methylethcathinone, mephedrone (4-methylmethcathinone), methedrone/bk-PMMA (methoxymethcathinone), MDPV (methylenedioxypyrovalerone), butylone/bk-MBDB (methylamino-1-(3,4-methylenedioxyphenyl) butan-1-one) and methylone/bk-MDMA (2-Methylamino-1-(3,4-methylenedioxyphenyl) propan-1-one).

 

“Prep-and-Shoot”: The Completely Automated Workflow for the Hydrolysis and Analysis of Urine Samples by LC/MS/MS

In this application note, a completely automated, 96-well plate format “Prep-and-Shoot” workflow including enzymatic hydrolysis, dilution and injection is described. A GERSTEL MultiPurpose Sampler (MPS) coupled to an AB SCIEX QTRAP® 4500 LC/MS/MS system was used for a fast enzymatic hydrolysis process (15 minutes), dilution and injection of urine samples. The procedure was applied to the analysis of multiple drug classes (e.g., opiates, opioids, benzodiazepines, muscle relaxants, hallucinogens) in urine. 

 

UHPLC Analysis Of Immunoglobulins With TSKgel® UP-SW3000 SEC Columns

Antibody therapeutics are enjoying high growth rates, the major areas of therapeutic application being cancer and immune/inflammation-related disorders including arthritis and multiple sclerosis. In 2013, six of the top ten best-selling global drug brands were monoclonal antibodies (mAbs) and more than 400 monoclonals were in clinical trials. The characterization of these complex biomolecules is a major challenge in process monitoring and quality control. The main product characteristics to be monitored are aggregate and fragment content, glycosylation pattern and charged isoforms.

 

Sensitive Determination of Polycyclic Aromatic Hydrocarbons in Tap Water

This application note demonstrates the sensitive and rapid determination of polycyclic aromatic hydrocarbons (PAHs) in tap water using the Agilent 1200 Infinity Series Online SPE Solution.

 

Extractables and Leachables Analysis of IV Bag Systems using Direct Thermal Extraction of the Materials and Stir Bar Sorptive Extraction of Aqueous Solutions coupled with Thermal Desorption Gas-Chromatography with Unit Mass and High Resolution Mass Spectrometric Detection

IV bag components were analyzed for extractables using direct thermal desorption/thermal extraction combined with a unit mass resolution GC/MSD system. The results were compared to those obtained for leachables by stir bar sorptive extraction of an aqueous simulant stored in the exact same type of IV bag, again combined with GC/MS determination of the leached compounds. In addition, the high resolution GC/Time of Flight (TOF) mass spectrometer was used to verify or disprove some of the MSD findings.

 

High resolution Saccharide and Polysaccharide Analysis using Small Particles

Polysaccharides are very important in nature, occurring in food (starches in rice, wheat etc.) and plants (cellulose). Some polysaccharides are also produced commercially (e.g. dextrans), which are manufactured through the fermentation of sugar solutions. These are higher molar mass polysaccharides. The PSS SUPREMA column with a reduced particle size of 5 μm offers a significant improvement in performance compared to traditional 10 μm materials and provides outstanding additional resolution, especially in the low molecular weight area, which is a major consideration when analysing oligomeric polysaccharides.

 

Comprehensive Analysis of Coffee Bean Extracts by GC×GC–TOF MS

This application note shows that BenchTOF time-of-flight mass spectrometers, in conjunction with GC×GC, provide a high-performance solution for screening for key aroma compounds in complex coffee extracts.

 

Monitoring Peracetic Acid (PAA) in a Beverage Bottling Facility

The importance of sanitary practices when it comes to processing and handling food and beverages cannot be overstated – long shelf lives and safe food depend upon completely hygienic conditions. There are many ways to disinfect a process line, generally using high heat, ozone (O 3), chlorinated or sulfonated compounds, but peracetic acid (PAA) is valued above most other chemical sanitizers in the food and beverage industry for the sanitization of new and recycled PET bottles. PAA is found to be harmless enough by the FDA to allow direct contact with meat, vegetables, and fruits.

 

Qualitative LC-MS/MS Analysis of 13 Food Allergens in a Single Injection on the QTRAP® 4500 System

A method is described using the Scheduled MRM™ Algorithm to detect multiple signature peptides corresponding to a variety of food allergens in bakery-product and raw food matrices.

 

Determination of choline in baby milk powder

Choline is biologically important for the biosynthesis e.g., of the neurotransmitter acetylcholine. Its concentration in baby milk powder is determined after microwave digestion. The separation is performed on a Metrosep C Supp 1 - 250/4.0 with subsequent conductivity detection after sequential suppression. Choline is well separated from standard cations.

 

Biogenics amines besides standard cations with suppressed conductivity detection applying a Dose-in Gradient

Biogenic amines are quality markers for food samples as e.g., fish and wine. Here, the simultaneous separation of standard cations, putrescine, cadaverine, and histamine is presented. The separation is performed on a Metrosep C Supp 1 - 250/4.0 applying a Dose-in Gradient with subsequent conductivity detection after sequential suppression.

 

Ammonium- sequential suppression with linear calibration

Ammonium determination with suppressed cation chromatography often suffers from non-linear calibrations. This is due to the conversion to ammonium hydroxide. Applying Metrohm sequential cation suppression yields ammonium hydrogen carbonate. Under these conditions, ammonium and the other standard cations show linear calibration curves (R better than 0.997).

 

Reproducibility of 10 ug/L injections after cation suppression

In cation chromatography with sequential suppression, cations are detected in their hydrogen carbonate form. The eluent – mainly nitric acid – is converted to carbonic acid. After decomposition of the latter, the carbon dioxide is removed by the CO2 Suppressor. The reduction of the baseline noise allows to reduce the detection limits and improves the reproducibility, even for very low concentrations. Here, the reproducibility for a 10 μg/L standard is shown.

 

Traces of lithium and sodium besides monoethanolamine in water-steam circuits of thermal power plants

Boiler feed water is the operating medium in thermal power plants. To suppress corrosion, the pH value of the feed water is adjusted with amines. Their addition has to be regularly controlled. Besides, the monitoring of the sodium concentration is crucial, since an increase probably points to infiltrating cooling water caused by a leak in the condenser. Ion chromatography with conductivity detection after sequential suppression is a powerful monitoring tool, especially when combined with the intelligent Preconcentration Technique and Matrix Elimination.

 

Alternative Carrier Gases for ASTM D7213 Simulated Distillation Analysis

Crude oil consists of thousands of different hydrocarbons that span a very wide volatility range. In order to efficiently produce quality finished products, refineries depend on simulated distillation (SimDist) analyses to characterize the composition of their crude feedstock prior to processing. SimDist is a gas chromatography (GC) technique that allows fast, reproducible, and easily automated determination of boiling point distribution of crude oil samples. Here we explore alternative carrier gas options for SimDist analyses and discuss their various benefits and drawbacks.

 

LC-MS/MS Analysis of Emerging Food Contaminants - Detection of Pesticide 1080 in Milk and Infant Formula using the SCIEX QTRAP® 6500+ System

Liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) is an ideal analytical technique to detect polar analytes in complex food samples. Here we present first results of method development to detect sodium fluoroacetate in milk and infant formula. The sample preparation protocol and LC conditions were adopted from the AOAC First Action Official Method 2015.03.

 

Automated Sample Preparation for Metabolomics Studies Using the Gerstel MPS Dual Head WorkStation - Part 2: Automated Lipid Fractionation Using Solid Phase Extraction

In metabolomics studies, large sample sets have to be analyzed to allow statistical differentiation of sample types. In a series of articles, we describe the use of the Gerstel MPS WorkStation for automated sample preparation applied to metabolomics studies. In a first part, an automated ultrasonic assisted extraction and filtration method was discussed. In this second part, an automated fractionation of lipid classes using solid phase extraction (SPE) is presented.

 

Traces of Lithium and Sodium besides Monoethanolamine in Water-steam Circuits of Thermal Power Plants

Boiler feed water is the operating medium in thermal power plants. To suppress corrosion, the pH value of the feed water is adjusted with amines. Their addition has to be regularly controlled. Besides, the monitoring of the sodium concentration is crucial, since an increase probably points to infiltrating cooling water caused by a leak in the condenser. Ion chromatography with conductivity detection after sequential suppression is a powerful monitoring tool, especially when combined with the intelligent Preconcentration Technique and Matrix Elimination.

 

Determination of Dimethylamine in Meropenem Applying Sequential Suppression

Meropenem is used to treat a wide variety of bacterial infections. It is known as a carbapenem-type antibiotic, and, as a ß-lactam antibiotic, it works by inhibiting the cell wall synthesis of bacteria. Dimethylamine is a precursor in meropenem production and thus occurs as an impurity in the final product. It is determined on a Metrosep C Supp 1 - 250/4.0 column with conductivity detection after sequential suppression.

 

A Determination of Veterinary Drug Residues in Milk Using Polymeric SPE and UHPLC-MS/MS Analysis

This application note outlines a multi-class, multi-residue method for the determination of 49 representative veterinary drugs in milk using a simple, solid-phase extraction (SPE) procedure and analysis by UHPLC-MS/MS. To achieve fast and simultaneous extraction of the various drug residues, a generic liquid extraction procedure using EDTA/acetic acid buffer is conducted prior to extraction on a polymeric SPE cartridge.

 

Time Saving, High Resolution GPC/SEC using Microcolumns and Optimized RI Detection

Efficient and fast separation for low molar mass polymers and proteins can be achieved using a combination of micro columns packed with smaller particles and optimized detectors. Although traditional analytical RI detectors, such as the SECcurity RI, profit from the higher resolution of micro columns, less peak broadening and higher resolution are the benefits that dedicated micro cell detection units offer.

 

Enhanced Separation and Identification of Fungicides and Other Components in Wine by Headspace SPME–GC×GC–TOF MS

This Application Note describes the use of solid-phase micro-extraction (SPME) coupled with GC×GC–TOF MS for the detection of trace-level fungicides and compounds responsible for undesirable attributes (‘organoleptic faults’) in wine. Of particular interest are the fungicides, which because of their trace levels are difficult to detect using conventional quadrupole GC–MS without resorting to selected ion monitoring mode.

 

Trace-level quantitation of tear gas lachrymators in complex matrices

This Application Note demonstrates the excellent performance of GC×GC coupled with a BenchTOF time-of-flight mass spectrometer for the forensic analysis of tear-gas lachrymators. Analysis of a lachrymator standard is first shown to provide robust quantitation, and this is followed by the detection of capsaicin and dihydrocapsaicin at trace levels in a complex extract from contaminated clothing.

 

Benefits of HPLC-ICP-MS Coupling for Mercury Speciation in Food

Mercury speciation in food analysis is necessary to fully estimate the toxic potential of this element to humans. HPLC-ICP-MS was used for the rapid analysis of mercury species in food samples, giving complete separation of four species of interest in less than three minutes. The method was tested on certified samples and demonstrated good Hg species recoveries compared to the certified values, where available.

 

Arsenic Speciation Analysis in Apple Juice using HPLC-ICP-MS with the Agilent 8800 ICP-QQQ

LC-ICP-QQQ was used to determine five arsenic species at low- and sub-μg/L concentrations in commercially available apple juice using. Detection limits between 10 and 20 ng/L (ppt) were obtained for all As species following a simple filtration and 2x dilution of the samples. Arsenic species, including the toxicologically relevant inorganic forms, were detected in all of the samples measured, although the concentrations of the different species varied among the brands.

 

Simultaneous Quantitation of Peptides and Phosphopeptides by capLC-ICP-MS using the Agilent 8800 Triple Quadrupole ICP-MS

ICP-QQQ was used for the trace measurement of phosphorus (P) in phosphopeptides and sulfur (S) in S-containing peptides following separation using capillary LC (capLC). The lowest absolute detection limits ever reported for the analysis of S- and P-containing species (11 fmol and 6.6 fmol, respectively) using LC-ICP-MS were achieved. The potential of the method for sensitive and simultaneous absolute quantitation of P- and S-containing peptides using non-specific standards is demonstrated.

 

Application of a New Capillary HPLC-ICP-MS Interface to the Identification of Selenium-containing Proteins in Selenized Yeast

An ICP-MS-assisted proteomic approach was used to identify Se-containing proteins present in selenized yeast. The insoluble Se-containing proteins were first separated by 2D gel electrophoresis then excised and digested with trypsin. The resulting peptides were analyzed by capillary HPLC-ICP-MS and then characterized by electrospray ionization (ESI-) MS/MS leading to the identification of glyceraldehyde-3- phosphate dehydrogenase-3 - the major Se-containing protein in selenized yeast.

 

Accurate Determination of Sulfur in Biodiesel using Isotope Dilution-Triple Quadrupole ICP-MS (ID-ICP-QQQ)

An accurate, sensitive and fast analytical method for the determination of low levels of sulfur (S) in organic matrices is described. Interferences on both 32S and 34S were eliminated by reacting the analyte ions with O2 and measuring the isotope-specific SO+ product ions at M + 16 amu using ICP-QQQ for isotope dilution purposes. The method is suitable for on-line species-unspecific isotope dilution quantification of S-containing materials via reverse phase HPLC-ICP-MS.

 

LC-ICP-MS Method for the Determination of Trivalent and Hexavalent Chromium in Toy Materials to Meet European Regulation EN71-3:2012 Migration of Certain Elements

Chromium normally exists as either trivalent or hexavalent Cr. While Cr(III) is an essential trace nutrient for human health, Cr(VI) is toxic. LC-ICP-MS was used to separate and determine Cr(III) and Cr(VI) in toy material to comply with the limits specified in European Standard EN71-3 (2012). The method achieved single digit ppt DL for both Cr species, exceeding the requirements specified in EU Toy Safety Directive (2009/48/EC).

 

Select-eV: The next generation of ion source technology

This Application Note describes Select-eV®, a new development in ion-source technology for GC–MS that allows the energy of electron ionisation to be reduced on a sliding scale from 70 eV to 10 eV without impacting sensitivity, simply by changing a parameter in the method.

 

Speciation of Inorganic Arsenic in Baby Rice Cereals using HPLC-ICP-MS

A survey of 31 baby rice cereals using HPLC-ICP-MS detected all arsenic species in all of the cereals tested – including highly toxic inorganic arsenic (iAs) species. The method used was specified the FDA Elemental Analysis Manual (EAM): Section 4.11 for the speciation of arsenic in baby rice cereals. The average percentage of iAs as a component of the average total arsenic in the baby rice cereals tested was 58.2%.

 

Rapid Determination of Five Arsenic Species in Polished Rice using HPLC-ICP-MS

Five arsenic species, including the toxicologically relevant inorganic forms As(III) and As(V), were determined in 4 minutes, with excellent sensitivity, accuracy and precision using an LC fitted with a reversed phase column coupled to an ICP-MS. Any potential interferences on As such as ArCl+ were removed using a single-cell gas mode (helium mode), speeding up the analysis. Inorganic arsenic species were detected in all of the twenty rice samples tested - at various concentrations.

 

Sub-ppb Detection Limits for Hydride Gas Contaminants using GC-ICP-QQQ

Hydride gas contamination of process chemicals used in the petrochemical and semiconductor industries is problematic. Increasing competition within the industry and evolving performance criteria are pushing specifications below the ppb level. ICP-QQQ with MS/MS allows accurate measurements of previously difficult elements such as S, P and Si in complex samples, while sensitivity is significantly increased. Compared to GC-ICP-MS with conventional quadrupole ICP-MS, GC-ICP-QQQ detection limits for silane, phosphine, hydrogen sulfide, and carbonyl sulfide were lower by a factor of 5 to 10 - in the ~200 ppt range for silane and ~15 ppt range for phosphine.

 

Comprehensive Characterisation of Essential Oil by GC×GC–TOF MS

This application note shows that BenchTOF time-of-flight mass spectrometers, in conjunction with GC×GC, provide a high performance solution for comprehensively screening the total composition of essential oils.

 

Extended Detection Limits for GC–TOF MS of Organotins using Select-eV Variable-energy Electron Ionisation

This application note demonstrates how the enhanced sensitivity and selectivity of the BenchTOF time-of-flight mass spectrometer with Select-eV variable-energy electron ionisation can provide ultra-trace-level quantitation of organotins in complex environmental extracts. The focus is on how Select-eV soft ionisation offers particular advantages in the analysis of organotin species, which undergo extensive fragmentation at conventional 70 eV ionisation energies, by producing simplified spectra with enhanced diagnostic ions.

 

Forensic Toxicology - Efficient Automated Drug Analysis

This article demonstrates the comprehensive automation of an SPE-GC/MS based analysis of serum and other matrices for opioids, cocaine and metabolites. The method is compared with a validated, partly-automated routine method.

 

Flavor Analysis - Tracking the Whole Range of Flavor Compounds

In this article, an overview is given of the Multi-Volatile Method (MVM), developed by GERSTEL application experts, which relies on a new analyte concentration technique and automated sample preparation to overcome the problems of determining all compounds from beverages in a single GC/MS run. 

 

Rapid and Accurate LC-MS/MS Analysis of Nicotine and Related Compounds in Urine Using Raptor™ Biphenyl LC Columns and MS-Friendly Mobile Phases

A rapid, accurate, and reproducible method was developed for high-throughput testing of nicotine, cotinine, trans-3'-hydroxycotinine, nornicotine, norcotinine, and anabasine in urine. Data show that a fast and highly efficient analysis of these basic compounds can be achieved with the Raptor™ Biphenyl column using standard low-pH, reversed-phase LC-MS mobile phases that are compatible with a variety of LC-MS instrumentation.

 

Investigation of Iron Polysaccharide Complexes by GPC/SEC Using RI- and UV-Detection

Dual-detection Gel Permeation Chromatography (GPC), also known as Size Exclusion Chromatography (SEC), provides an easy and effective way to measure the molar mass distribution and the amount of free, unbound polysaccharide of iron polysaccharide complexes. 

 

Comprehensive Metabolite Identification – A One-Stop Solution

The determination of metabolic stability and the accurate prediction of major human metabolites are critical for the optimization of drug candidates. Analysis of HepatoPac® co-cultured hepatocytes using SWATH™ Acquisition on a TripleTOF® 6600 System delivered a one-stop solution for qual/quant across multiple species in a single experiment.

 

Oxyhalides Besides Standard Anions in Swimming Pool Water

Swimming pool water needs to be disinfected thoroughly. Often ozone is used. As a result of this strong oxidation, oxyhalides may build up and need to be analyzed. Here, the separation and determination of oxyhalides besides standard anions is performed on a Metrosep A Supp 5 - 250/4.0 column with subsequent sequential suppression followed by conductivity detection.

 

Characterization Studies of PEGylated Lysozyme

PEGylation is a common practice to prolong serum half-life and improve pharmacokinetics of a drug. 

 

MAb Aggregate Detection – Analytical HIC as an Orthogonal Chromatographic Approach

Due to the hydrophobic nature of mAb aggregates, analytical hydrophobic interaction chromatography (HIC) can resolve the different aggregate species and can serve as a back-up method for SEC based aggregate analysis. 

 

Fast Analysis of IgG Charge Heterogeneity by Ion Exchange Chromatography

This application note presents the analysis of mAb charge heterogeneity by cation exchange chromatography on TSKgel STAT columns. 

 

UHPLC Glycosylation Analysis with TSKgel Amide-80 2 μm HILIC Columns

Hydrophilic interaction liquid chromatography (HILIC) is a well-recognized technique that effectively separates and quantifies isolated glycans.

 

EPA Method 545: Determination of Cylindrospermopsin and Anatoxin-a in Drinking Water by Aqueous Direct Injection and LC/MS/MS

This application note describes a direct aqueous injection and liquid chromatography tandem mass spectrometry (DAI-LC/MS/MS) method for the determination of cylindrospermopsin (hepatotoxin) and anatoxin-a (neurotoxin) in drinking water under EPA Method 545.

 

Analysis of mAb and Protein Aggregates using a Novel SEC Column

This application note shows the superior resolving power of the TSKgel UltraSW Aggregate column for the analysis of monoclonal antibody and metalloprotein aggregates formed under forced denatured conditions, including acid and thermal denaturation.

 

UHPLC Analysis of IgG with TSKgel UP-SW3000 SEC Columns

The standard method used in biopharmaceutical QC for mAb aggregate and fragment analysis is size exclusion chromatography (SEC).

 

LC-MS/MS Analysis of Emerging Food Contaminants - Detection of Peanut and Almond Allergens in Spices

LC-MSMS Analysis of Emerging Food Contaminants - Detection of Peanut and Almond Allergens in Spices

Here we present a method to detect the presence of peanut and almond in spices. Samples were extracted and then the allergenic proteins were reduced, alkylated and digested using trypsin. The extract containing peptides from the digested proteins were filtered and analyzed by LC-MS/MS using a reverse phase chromatography and positive polarity electrospray ionization (ESI).

 

Simultaneous Quantitative Analysis of Total Catecholamines and Metanephrines in Urine Using 500 MG CLEAN UP® CCX2 and LC-MS/MS

Catecholamines are hormones produced in the interior region of the adrenal glands. These hormones function in the control of heart rate, metabolism and blood pressure. In this application note, UCT's CLEAN UP® CCX extraction columns along with a Selectra® PFPP HPLC column are used for sample preparation and analyte separation.

 

Extraction of THC, Hydroxy-THC and Carboxy-THC from Whole Blood Using ISOLUTE® SLE+ Prior to GC/MS Analysis

This application note describes the extraction of Δ9-THC, 11-hydroxy- Δ9-THC and 11-nor-9-carboxy-THC  from whole blood matrix, prior to GC/MS analysis.

 

Extraction of 11-nor-9-carboxy-tetrahydrocannabinol from Hydrolyzed Urine by ISOLUTE® SLE+ Prior to GC/MS Analysis

This application note describes the extraction of 11-nor-9-carboxy-THC from a urine matrix, prior to GC/MS analysis. 11-nor-9-carboxy-tetrahydrocannabinol (carboxy-THC; THC-COOH) is the primary metabolite of THC. In urine, 80% of THC-COOH is present in the form of its glucuronide metabolite. Therefore, to effectively quantitate the THC-COOH, urine is hydrolyzed before extraction. This application note describes optimized extraction of urine samples prepared by either enzymatic or base hydrolysis.

 

Acarbose Analysis by HPLC

Acarbose is used to treat type 2 diabetes. By using COSOMSIL Sugar-D, which is designed for saccharide analysis, high-resolution separation of Acarbose and its impurities was obtained. Furthermore, COSMOSIL Sugar-D was more durable than the conventional NH2 column.

 

Analysis of Vitamins D2 and D3 by Cholesterol-Bonded UHPLC Column

Structurally similar compounds such as vitamins D2  and D3 are difficult to analyze with alkyl group bonded materials. COSMOCORE Cholester’s unique cholesterol-based stationary phase offers superior molecular shape selectivity, resulting in better separation for vitamins D2  and D3.

 

Separation of Polar Compounds by Reversed-Phase HPLC Column

Due to the complex retention mechanisms of HILIC mode, such as hydrophilic partitioning and electrostatic interactions, all HILIC columns do not retain polar compounds in a similar manner. This poses a common challenge in HILIC method development: identifying the most suitable column to use. Nacalai Tesque recently developed a novel pentabromobenzyl stationary phase to separate highly polar molecules in reversed phase conditions. This column may offer simpler forward method development for separation of polar compounds.

 

Cannabinoids Analysis by Cholesterol-Bonded UHPLC Column

Four cannabinoids, CBD, CBN, Δ9-THC, and Δ8-THC were analyzed by core-shell HPLC columns. The C18 core-shell column produced co-eluting peaks of Δ9-THC and Δ8-THC. COSMOCORE Cholester is a core-shell HPLC column that has similar hydrophobicity to C18. The rigid cholesterol group provides it with higher steric selectivity to resolve the Δ9-THC and Δ8-THC peaks.

 

Fatty Acid Methylation Kits (General Purpose and for Glycerides) for GC

Nacalai Tesque's Fatty Acid Methylation Kits offer significant improvement over conventional methods for methylating fatty acids prior to GC analysis. The general-purpose kit can methylate in 1.5 hours at 37 °C and is suitable for free fatty acids, glycerolipids and sterol esters. The glyceride kit can methylate fatty acids from glycerides at room temperature in less than 1 minute.

 

COSMOSIL SFC Columns

Supercritical Fluid Chromatography (SFC) has become more attractive because it offers some advantages over HPLC, such as high speed, unique selectivity and environmentally friendly separations. Many conventional normal-phase stationary phases, such as diol, amino and cyano, have been used for SFC applications. However, these phases present limitations for separations. Nacalai Tesque has developed 3 SFC columns (3-Hydroxyphenyl, Quinoline and 2-Pyridinyl) to enhance the capability of SFC separations.

 

Comprehensive Detection and Identification of Synthetic Cannabinoids using the Toxtyper Platform

For nearly a decade synthetic cannabinoids are among the most prevalent new emerging psychoactive substances. Hyphenated mass spectrometry (MS) is the method of choice and state-of-the-art for developing analytical methods to detect and identify synthetic cannabinoids in either biological matrices or seized material. In this application note, the ToxtyperTM: an LC-MSn library-based solution that is conveniently applied to address these analytical challenges, is presented.

 

Analysis of Nicotine and Impurities in Electronic Cigarette Solutions and Vapour

Electronic cigarettes (e-cigarettes) are growing in popularity exponentially. Despite their ever-growing acceptance, relatively little work has been done to characterize their vapour. To date, the majority of e-cigarette research has focused on characterizing the solutions, which are ultimately vaporized for the end user to inhale. The current study focused on developing a complete analytical package for the quick and simple analysis of electronic cigarette solutions and vapour to determine nicotine content and impurity profiles.

 

Paracetamol in Tablets with Fully Automated Sample Preparation using the 815 Robotic Soliprep for LC

Metrohm presents a new application describing the fully automated determination of paracetamol in tablets with ion chromatography and an 815 Robotic Soliprep LC for sample preparation.

 

Extraction of Anabolic Steroids from Horse Urine Using ISOLUTE® SLE+ Prior to LC-MS/MS Analysis

This application note describes a Supported Liquid Extraction (SLE) method for extraction of ethylestrenol and stanozolol from both gelding and filly horse urine prior to LC-MS/MS analysis. The method from Biotage shows high reproducible analyte recoveries.

 

Polydextrose in Biscuits with IC-PAD in Line to AOAC 2000.11

Metrohm has developed an application for the determination of polydextrose in biscuits in accordance with AOAC 2000.11. Polydextrose is a low calorie synthetic polymer of glucose. It is an accepted additive for food. Polydextrose is extracted from food samples with hot water and centrifuged. Subsequent digestion removes maltooligomers and fructans. Finally, polydextrose is quantified by anion-exchange chromatography followed by pulsed amperometric detection.

 

EPA Method 538: Determination of Selected Organic Contaminants in Drinking Water by Aqueous Direct Injection and LC/MS/MS

This application outlines a direct aqueous injection-liquid chromatography/tandem mass spectrometry (DAI-LC/MS/MS) method for the determination of 11 selected organic contaminants in drinking water, including methamidophos, acephate, aldicarb sulfoxide, oxydemeton methyl, dicrotophos, aldicarb, diisopropyl methylphosphonate (DIMP), fenamiphos sulfone, fenamiphos sulfoxide, thiofanox, and quinoline. Dicrotophos, oxydemeton methyl, methamidophos, and acephate are UCMR4 compounds.

 

Enhanced Separation and Identification of Fungicides and Other Components in Wine by Headspace SPME–GC×GC–TOF MS

This application note describes the use of solid-phase micro-extraction (SPME) coupled with GC×GC–TOF MS for the detection of trace-level fungicides and compounds responsible for undesirable attributes (‘organoleptic faults’) in wine. Of particular interest are the fungicides, which because of their trace levels are difficult to detect using conventional quadrupole GC–MS without resorting to selected ion monitoring mode.

 

Sophisticated Antibody Analysis by GPC/SEC Multi-chrome Light Scattering

A multidetection GPC/SEC method including UV, RI and light scattering can be used for the simultaneous determination of aggregate content of monoclonal antibodies and antibody fragments using a single column set.

 

Quantitation of 250 Pesticides in Fruit Juices with Positive/Negative Switching LC-MS/MS

Quantitation of 250 Pesticides in Fruit Juices with PositiveNegative Switching LC-MSMS

A number of factors are increasing the strain on modern food testers. The increased variety of pesticides employed in global crop production, along with the expanding international export market, has seen the quantity of samples and monitored analytes rise substantially. To continue to meet productivity targets, contract and QC labs around the world are in need of detection methods that reduce the analytical cycle time while delivering enhanced sensitivity, reliability and robustness.

 

Automated Derivatization, SPE Cleanup and LC-MS/MS Determination of Glyphosate and Other Polar Pesticides

Glyphosate and glufosinate are widely used herbicides and, thus, there is an interest in the reliable and sensitive determination of glyphosate in water and food. These pesticides are difficult to extract and analyse because of their high polarity. Here we describe an automated workflow for the FMOC-derivatization, sample cleanup, and LC-MS/MS detection using a GERSTEL Multi Purpose Sampler (MPS) 2XL configured with an online solid phase extraction (SPEXOS) module coupled to an AB SCIEX QTRAP® 4500 system for the identification and quantitation of glyphosate, its major metabolite AMPA, and glufosinate in water and food samples.

 

Reduction of Matrix Effects using LC-MS/MS with Online Extraction for Quantitation of Antibiotics in Milk

A study was carried out using the Bruker EVOQ Elite liquid chromatography mass spectrometer (LC-MS/MS) with an online extraction (OLE) option to quantify 8 antibiotics in milk. The milk matrix clean-up was performed online using an innovative UHPLC integrated with a binary pump and one loading pump. The EVOQ Elite with OLE showed a significant reduction of matrix effects and excellent linearity, with online extraction providing an effective, timesaving approach for clean up.

 

Comprehensive Detection and Identification of Synthetic Cannabinoids using The Toxtyper platform

For nearly a decade synthetic cannabinoids are among the most prevalent new emerging psychoactive substances. Herbal mixtures containing synthetic cannabinoids are readily available over the Internet. These products are marketed as incense, plant-fertilizer or car-perfume and are sold as an alleged legal alternative to cannabis products to circumvent narcotics laws and drug-testing. Accordingly, these products are of special interest to consumers who do not have easy access to cannabis as well as those that are subject to drug testing (e.g. workplace drug testing candidates, patients in drug rehabilitation centres or forensic clinics).

 

Adopting Forensic Analyses to Specific Lab Needs – Identifying Psychotropics in Serum Using the Toxtyper Open Library Concept

Various instrument types and LC-MS approaches have been explored in an attempt to develop a comprehensive analysis method for detecting and definitely identifying as many compounds as possible in a single run. However, everyday analyses often require the detection of a defined set of substances (for example, hypnotics in cases of drug facilitated assault (DFA). The aim of this project was to develop an analysis method for psychotropic medical drugs based on the Toxtyper™ open library concept.

 

Improved Determination of Allergenic Fragrances in Detergents and Personal Care Products in Multiple Reaction Monitoring GC-MS/MS

A study was carried out using the Bruker SCION TQ gas chromatography triple quadrupole mass spectrometer in multi reaction mode (MRM) to screen for allergenic fragrances within cleaning fluids and personal care products (PCPs). Compound based scanning (CBS) was used to target compounds listed in EU Directive No. 76/768/EC.

 

Analysis of Persistent Organic Pollutants (POPs) in Silver Gull Eggs Using the Scion™ TQ GC-MS/MS System

The use of whole seabird egg for environmental contaminant testing is well established. In this study, the levels of organochlorine pesticides (OCPs), a significant group of persistent organic pesticides (POPs), were investigated in the eggs of silver gulls (Chroicocephalus novaehollandiea ). The components were extracted using a modified QuEChERS method. Matrix matched standards were prepared using extracted yolk, albumen and eggshell from commercially available chicken eggs.

 

An evaluation of hydrogen as a carrier gas in the analysis of the halogenated pesticide-herbicide mixture listed in US EPA Method 551.1

Method 551.1 contains a list of analytes which includes: 12 commonly observed chlorination disinfection by-products, 8 commonly used chlorinated organic solvents and 16 halogenated pesticides and herbicides.

 

A Fast and Robust HPLC Separation of Bile Acids and Their Conjugates with Ascentis® Express C18

The quantitation of plasma bile acids by tandem mass spectrometry MS/MS presents an analytical challenge. To enable separation, several orthogonal HPLC stationary phases were screened for selectivity. The best separation was achieved with an Ascentis Express C18 analytical column based on Fused-Core® technology.

 

Forced Degradation Analysis of Omeprazole Using CORTECS 2.7 µm Columns

Omeprazole is a basic compound that acts as a proton pump inhibitor used in the treatment of acid reflux and heartburn. This API is also unstable at low pH. Forced degradation under acidic conditions is needed to identify/characterize by-products formed under such conditions. CORTECS 2.7 µm columns allow for high resolution between peaks in complex mixtures such as forced degradation samples.

 

Prepare Olive Oil Samples for Pesticide Residue Analysis in Half the Time With a Fraction of the Solvent Using dSPE

In this application the extraction and cleanup of pesticide residues  from olive oil samples is shown using a dSPE procedure. This is shown to be twice as fast as GPC, with only a fraction of the solvent required for conventional SPE. The efficiency of the method is demonstrated  as well as the capabilities of a method-specific analytical column.

 

Analysis of Synthetic Cannabinoids from Whole Blood for Forensic Toxicology Using Ostro Sample Preparation Plates and CORTECS UPLC Solid-Core Columns

This application note details a strategy for the successful extraction and analysis of representatives of several different classes of synthetic cannabinoids from whole blood samples for forensic toxicology. Twenty-two synthetic cannabinoids and metabolites were extracted from whole blood samples using a rapid and universal sample preparation strategy that provides effective sample cleanup and is generic enough to use on a variety of compounds with different chemical properties.

 

Extraction of NSAIDs from Plasma Using ISOLUTE® SLE+

A utomated sample preparation using the Biotage®  Extrahera™ was compared to an equivalent manual  method utilizing a vacuum manifold. A selection  of non-steroidal anti-inflammatory drugs (NSAIDS)  were extracted from pooled stripped plasma using a  supported liquid extraction procedure.

 

Analysis of Pesticides in Food Samples Using the SCIEX Triple Quad™ 3500 System

Analysis of Pesticides in Food Samples Using the SCIEX Triple Quad 3500 System

Modern analytical techniques, such as LC-MS/MS allow the screening for hundreds of pesticide residues in food samples quickly, efficiently, and with excellent sensitivity and selectivity to meet global food trade guidelines and regulations. This application note describes a method using QuEChERS extraction and the SCIEX Triple Quad™ 3500 system.

 

Simultaneous Analysis of Chloramphenicol and Tetracycline Antibiotics in Food Samples Using the AB SCIEX Triple Quad™ 3500 System

Simultaneous Analysis of Chloramphenicol and Tetracycline Antibiotics in Food Samples Using the AB SCIEX Triple Quad 3500 System

Utilizing liquid chromatography with tandem mass spectrometry (LC-MS/MS) to analyze for antibiotic residues in a food samples offers many benefits to routine food testing labs, including the ability to screen for many compounds at once, the selectivity to meet regulatory guidelines, and the sensitivity to reduce sample  preparation time to get to results faster. Here we present a method using the AB SCIEX Triple Quad™ 3500 system for the detection of  chloramphenicol and tetracyclines.

 

Time Saving, High Resolution GPC/SEC using Micro Columns and Optimized RI Detection

Efficient and fast separation for low molar mass polymers and proteins can be achieved using a combination of micro columns packed with smaller particles and optimized detectors. Although traditional analytical RI detectors, such as the SECcurity RI, profit from the higher resolution of micro columns, less peak broadening and higher resolution are the benefits that dedicated micro cell detection units offer.

 

Combined Determination of 1,4-Dioxane and Nitrosamine Contaminants in Drinking Water

The method described here uses the same coconut charcoal sorbent solid phase extraction (SPE) cartridges and dichloromethane eluent recommended in EPA Methods 522 and 521 to concentrate 0.50 L water samples to 10 mL extracts. However, both the extraction and instrumental analysis portions of EPA Methods 522 and 521 have been combined by analysing a single quantitatively collected SPE tube extract for both 1,4-dioxane and nitrosamines during a single chromatographic run.

 

Rapid Quantitation of Substance P in Plasma Using Differential Mobility Spectrometry and Microflow Liquid Chromatography

A selective and sensitive strategy for high throughput peptide quantification is presented by coupling DMS (Differential Mobility Spectrometry) technology with μLC/MS/MS analysis. Substance P is an 11 amino acid neuropeptide that is known to modulate neural responses primarily associated with pain perception. A fast and robust method is described to detect and quantitate Substance P in protein precipitated plasma. 

 

Sunscreen Testing According to COLIPA 2011/FDA Final Rule 2011 Using UV/Vis LAMBDA Spectrophotometers

Sunlight striking the Earth is composed of 50% infrared, 40% visible and 10% UV. Of the UV component, 9.5% is UVA and 0.5% is UVB. Research has shown that sun exposure can have both acute and chronic consequences for the skin. A number of methods, developed in Europe, Australia, Germany, UK, and the United States (ISO, AS/NZS, DIN, UK, FDA) based on both in vivo and in vitro techniques have been proposed together with different ways to label the level of UVA protection. Unfortunately, there has been little synchronization of the methods being developed worldwide for uniform labelling of UVA effectiveness. The two protocols to be discussed in this paper are COLIPA 2011 and the FDA Final Rule 2011.

 

POSTER - Monitoring odorous sulfur compounds by thermal desorption TD-GC-MS

A number of volatile organic compounds (VOCs) – and sulfur compounds in particular – are a challenge for the analyst because they can decompose at the high temperatures used by GC-MS analytical equipment.

 

POSTER - Comprehensive material emissions profiling by TD-GCxGC-TOF MS

This poster describes a holistic approach to material emissions profiling, by combining thermal desorption with GC×GC–TOF MS and novel ion source technology.

 

POSTER - Advances in tube sampling technology - tube and sample data tracking

This poster describes the implementation of Tube TD this technology and discusses its place within the modern analytical laboratory.

 

POSTER - Monitoring siloxanes in biogas using thermal desorption tube sampling

Thermal desorption TD) is an ideal technique for the analysis of trace-level siloxanes in biogas. It provides both analyte concentration and efficient transfer/injection the GC analytical system.

 

POSTER - New advances in environmental air monitoring

This poster describes a cryogen-free, analytical system designed to offer flexibility of sampling methodology, fully compliant with US EPA Methods TO-15 (canisters) and TO-17 (sorbent tubes).

 

Analysis of Aroma Compounds in Edible Oils by Direct Thermal Desorption GC/MS using Slitted Microvials

This application note describes the direct thermal desorption of desirable and undesirable aroma compounds from edible oils. The oil sample is placed in a microvial from where it is directly thermally desorbed using a GERSTEL Thermal Desorption Unit (TDU). Volatile compounds are transferred  to the GC/MS system while leaving the non-volatile oil matrix behind in the microvial, preventing it from reaching and contaminating the GC inlet and the GC column.

 

Automated Sample Preparation and Analysis Workflows for Pesticide Residue Screenings in Food Samples using DPX-QuEChERS with LC/MS/MS

QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation methods have been developed to help monitor pesticides in a range of food samples. These methods require many manual steps, such as shaking, centrifugation, and dispersive SPE, making it a quite labor-intensive process.

 

Automated Derivatization, SPE Cleanup and LC/MS/MS Determination of Glyphosate and Other Polar Pesticides

Glyphosate and glufosinate are widely used herbicides and, thus, there is an interest in the reliable and sensitive determination of glyphosate in water and food. These pesticides are difficult to extract and analyze because of their high polarity.

 

Development of an Automated Sample Preparation and Analysis Workflow for Mycotoxin Residues in Different Food Matrices

In this application note, we describe a completely automated sample preparation workflow for the extraction and screening of multi-mycotoxin residues in different food matrices (corn, wheat) by LC/MS/MS. The extraction and cleanup was performed using a GERSTEL MultiPurpose Sampler (MPS XL) followed by LC/MS/MS determination using an AB SCIEX QTRAP® 4500.

 

High-Speed Quantitative Analysis of Antiepileptic Drugs Using Triple Quadrupole LC/MS/MS

This data sheet illustrates high-speed quantitative analysis of 16 anti-epileptic drugs (AEDs) using the Shimadzu UFMS Triple Quadrupole Mass Spectrometer, LCMS-8050.

 

LC-MS/MS Screening of 64 New Psychoactive Substances Using Dried Blood Spots

LC-MSMS Screening of 64 New Psychoactive Substances Using Dried Blood Spots

A robust, fast, sensitive and specific LC-MS/MS screening method for the determination of 64 new psychoactive substances in dried blood spots (DBS) has been developed and validated using an AB SCIEX QTRAP® 5500 LC/MS/MS System.

 

Fast Nevirapine Impurity Profiling Using UHPLC-DAD

Here we report optimization of the United States Pharmacopeia HPLC-UV approach to determine nevirapine and its impurities by using a state of the art gradient UHPLC-UV method.

 

The Vanquish Platform: Major Improvement in Throughput and Resolution of Xanthones in Mangosteen Pericarp

This application note describes an improved method to resolve many different analytes within a mangosteen pericarp sample in a finite time period with improved throughput, better resolution and enhanced peak capacity using the Vanquish UHPLC platform.

 

Simultaneous Determination of Amlodipine and Its Counterion Besylate by HPLC

This study focuses on an HPLC method to simultaneously separate the API and counterion of the drug substance amlodipine besylate.

 

Separation of Papain Digests of Oxidized Monoclonal Antibodies

This study shows that the ProPac HIC-10 column can resolve Fab and Fc fragments generated by papain digestion, as well as oxidized Fab/Fc from native Fab/Fc.

 

Separation of Intact Monoclonal Antibody Sialylation Isoforms by pH Gradient Ion-Exchange Chromatography

This study shows that pH-gradient-based strong cation exchange chromatography on the Thermo Scientific™ ProPac™ SCX-10 column can provide excellent resolution for MAb charge variants. Compared to routine isoelectric focusing methods, this method is more convenient and straightforward for protein quality control.

 

Product Authentication and Adulteration Determination Using a Novel Spectro-Electro Array Platform

A gradient HPLC spectro-electro array platform combines the universality of diode array detection with the selectivity and sensitivity of coulometric electrode array electrochemical detection.

 

Determination of Dicyandiamide in Milk Powder

Dicyandiamide is a compound used by farmers to minimize the environmental impact of livestock on land. Dicyandiamide reduces the rate at which soil microbes convert ammonia from animal urine into nitrates and nitrous oxide, thus slowing nitrate leaching from the pasture.

 

Determination of Carbonyl Compounds in Workplace Air

All 13 carbonyl compounds listed in CARB 1004, ISO 16000-3, U.S. EPA Compendium Method TO-11A, and the Chinese HJ/T 400-2007 are well resolved within 15 min on a Thermo Scientific™ Acclaim™ Carbonyl RSLC column using an ammonium acetate/acetonitrile mobile phase.

 

Comprehensive Neurochemical Profiling of Brain Tissue Samples

A new, modular, four-channel electrochemical array detector makes profiling biogenic amines and acid metabolites in brain tissue samples using UHPLC easier and faster.

 

Extraction of Acrylamide from Coffee and Potato Chips (Crisps) using Supported Liquid Extraction (SLE) prior to LC-MS/MS Analysis

Acrylamide analysis has increased in recent years due to its neurotoxic and carcinogenic properties. This poster demonstrates a novel, sensitive, cost effective and rugged method for the analysis of acrylamide in coffee and potato chips (crisps) using supported liquid extraction prior to LC-MS/MS analysis.

 

Fully Automated SPE-GC/MS Determination of Δ9-Tetrahydrocannabinol (THC) and its Metabolites in Serum Samples

This note presents a fully automated analysis system for the determination of Δ9-tetrahydrocannabinol (THC) and its metabolites in blood serum. Automation is based on the GERSTEL MultiPurpose Sampler (MPS) equipped for solid phase extraction (GERSTEL SPE) and a module for automated eluate evaporation (GERSTEL MultiPosition Evaporation Station, mVAP).

 

Automated Hydrolysis, DPX Extraction and LC/MS/MS Analysis of Pain Management Drugs from Urine

This study shows how a typical enzymatic hydrolysis procedure can be easily automated using a GERSTEL MultiPurpose Sampler(MPS), combining an automated extraction and clean-up procedure with introduction to the LC/MS/MS, in order to provide high throughput analysis of common pain management drugs.

 

Rapid Cleanup and Comprehensive Screening of Pain Management Drugs in Urine using Automated Disposable Pipette Extraction and LC-MS/MS

This study focuses on the automated extraction of small volumes of urine samples (< 500 μL) using disposable pipette extraction (DPX) for the comprehensive screening for pain management drugs by LC-MS/MS. Using a GERSTEL MPS autosampler, DPX extractions of hydrolyzed urine were performed, using a reversed phase (DPX-RP-S) sorbent.

 

Comprehensive Automation of the SPE-GC/MS Analysis of Opioids, Cocaine and Metabolites from Serum and Other Matrices

Analysing blood serum for opioids, cocaine and metabolites is a routine task in forensic laboratories. The most commonly used methods involve several manual or partly-automated sample preparation steps such as protein precipitation, solid-phase extraction, evaporation and derivatization followed by GC/MS or LC/MS determination. In this study a comprehensively automated method is compared with a validated, partly-automated routine method.

 

InertSustainTM C18

This application note explores the use of InertSustainTM C18. Tailing of peaks or adsorption of peaks can be experienced when a column has residual adsorption sites. Such phenomenon would not be observed on InertSustain as the silanols are completely end-capped, having a neutral silica surface. 

 

Fast and Simple Free fatty acids Analysis Using UPC2/MS

Fatty acids both free form and as part of complex complex lipids, play a number of key roles in metabolism. This application demonstrates the separation of free fatty acid (FFA) species based upon chain length and number of double bonds. 

 

Improved Recoveries and Lower Background for the Analysis of PAHs in Olive Oil

A recent survey implemented by Supelco revealed that 58% of analytical chemists in the food industry find the analysis of compounds in fatty matrices to be highly problematic. Lipid interferences can produce elevated detection limits, contamination of LC and GC systems, and ultimately decrease instrument and column lifetime.

 

Comprehensive material emissions profiling by TD–GC×GC–TOF MS

This poster describes a holistic approach to material emissions profiling, by combining thermal desorption with GC×GC–TOF MS and novel ion source technology to provide both enhanced separation and extended limits of detection for confident identification of a wide range of target compounds in a single analysis.

 

Enhanced screening of environmental pollutants in complex matrices by GC×GC–TOF MS with variable-energy electron ionisation

This poster shows the suitability of this innovative analytical platform for environmental investigations, using both target-focused studies as well as non-targeted routines for screening for the presence of emerging contaminants in two different, complex matrices.

 

Spot the difference: Novel software developments for comparative analysis of complex mixtures

This poster describes the innovative ChromCompare® comparative analysis molecular ion and a reduction in the number and relative intensity of fragment ions. 

 

Enhanced aroma profiling by GC–TOF MS with selective ionisation

This poster demonstrates the use of GC–TOF MS for aroma profiling of wine, with revolutionary variable-energy electron ionisation to provide enhanced molecular ions and reduced fragmentation to aid speciation of challenging compounds.

 

Select-eV: Increasing dimensionality in GC×GC–TOF MS

This poster provides an introduction to Select-eV, as applied to GC×GC–TOF MS analyses within a range of applications, from petrochemical analyses to environmental monitoring.

 

Qualitative and Quantitative Analysis of ß-carotene Using UPC2

Carotenoids are natural pigments synthesized by plants and some microorganisms. For animals and humans, carotenoids play an important part in vision. In this application note fast separations of three common carotenoids are described by UPC2 in less than 2 minutes.

 

Evolved Surface Silica

InertSustain employs a radically new type of silica, in which the surface of the silica is uniquely modified, enabling precise control of the silica properties and adsorption sites and silanol distribution are strictly controlled.

 

Exceptional Low Bleed Increases Detection Sensitivity

Baseline drift can be produced by many different causes, and bleed from columns is one of major cause.

 

High Inertness, High Plate Count and Low Column Backpressure

GL Sciences is the first company in the world who chromatographically emphasized the importance of the silica-gel purity and established a successful manufacturing process.

 

Rapid Re-equilibration Even with Gradients

InertSustainSwiftTM C18 columns are designed to enhance your High Throughput strategy by allowing rapid re-equilibration even with gradients.

 

Suitably Controlled Retentivity for High Throughput

InertSustainSwiftTM C18 columns are designed to enhance your High Throughput strategy by controlling pore size, 20 nm and surface area,

 

Separation of Statistic MMA-MAA Copolymers using Gradient SEC

Isocratic GPC/SEC is a powerful tool to separate macromolecules based on their hydro-dynamic volume. In case of homopolymers, GPC/SEC allows the fast, precise and easy determination of the complete molar mass distribution.

 

Safely convert your GC from helium to hydrogen carrier gas

Helium is running out and worldwide demand is exceeding current production levels. This global shortage means that not only are prices going through the roof, rationing is taking place to ensure that areas such as healthcare take priority.

 

Extraction of T3, rT3 and T4 from Serum Using EVOLUTE® EXPRESS AX Plates Prior to LC-MS/MS Analysis

The method described in this application note demonstrates selective extraction of the thyroid hormones T3, rT3 and T4 from serum. 500 μL of serum was extracted using the EVOLUTE EXPRESS AX 30mg fixed well plate format.

 

Automated Hydrolysis, DPX Extraction and LC/MS/MS Analysis of Pain Management Drugs from Urine

This study shows how a typical enzymatic hydrolysis procedure can be easily automated using a GERSTEL MultiPurpose Sampler(MPS), combining an automated extraction and clean-up procedure with introduction to the LC/MS/MS, in order to provide high throughput analysis of common pain management drugs.

 

Analysis of THC and an Extended Metabolite Suite from Oral Fluid Using ISOLUTE® SLE+ Supported Liquid Extraction Columns Prior to LC-MS/MS

The method described in this application note achieves high recoveries of THC and an extended suite of common metabolites in oral fluid from Quantisal™ oral fluid collection devices using ISOLUTE SLE+.

 

Effectiveness of Metabolomics Research Using GC / Quadrupole Mass Spectrometer with High-Sensitivity and High-Speed Scanning

GC/MS has been recognized as a core technology for metabolomics research for the comprehensive analysis of low-molecular weight compounds in living organisms, and is widely used for biomarker discovery and quality assessment.

 

Extraction of Antiepileptic Drugs from Oral Fluid Using ISOLUTE SLE Prior to LC-MS/MS Analysis

This application note describes the extraction of neutral and zwitterionic antiepileptic drugs from fortified oral fluid using ISOLUTE SLE in a 96-well plate format.

 

Molecular Weight Determination of Gelatin

Reproducible and easy-to-use GPC/SEC analysis for all types of Gelatins can be done using a SECcurity GPC system and PROTEEMA columns. Exact sample preparation, following a strict protocol, and the choice of the proper solvent is a crucial step for successful analysis. Determination of the molar mass distribution and the molar mass averages can be done using PSS WinGPC Software. A very comprehensive characterization for multimodal samples, like Gelatins, can be done using WinGPC multi area evaluation

 

Extraction of 1, α25-di-OH Vitamin D2, 1, α25-di-OH Vitamin D3, 25-OH Vitamin D2 and 25-OH Vitamin D3 from Serum Using ISOLUTE SLE+ Prior to LC-MS/MS Analysis

This application note describes a simple, clean and efficient Supported Liquid Extraction (SLE) protocol for the simultaneous extraction of 25-OH and 1, α25 di-OH-vitamin D2 and D3 metabolites from serum prior to LC-MS/MS analysis.

 

Excellent LC-MS Separation of Penicillins and Cephalosporins Using Ultra IBD Columns

Excellent LC-MS Separation of Penicillins and Cephalosporins Using Ultra IBD Columns

Antibiotics are the most widely used medications in the world. Whether by prescription, addition to animal feed stocks, or use of cleaning agents, everyone in the civilized world is either directly or indirectly exposed to antibiotics in daily life.

 

Merck Millipore Applications for Matrix-rich Food Samples

With the current focus on food analysis there is an increasing need for new analytical methods that are able to cope with a large number of analytes in complex matrices. With their high tolerance for complex sample matrices, monolithic columns are the preferred choice for “dirty” sample analysis.

See the possibilities for food safety and food quality control.

 

EMD Millipore Applications for UHPLC

Guidelines for high throughput separations – Applications for UHPLC with Chromolith® columns.

 

EMD Millipore Application Collection for Chromolith® HighResolution

View a selection of applications with Chromolith® HighResolution and learn how it can support your daily work in the lab.

 

Merck Millipore Applications for UHPLC

Guidelines for high-throughput separations – Applications for UHPLC with Chromolith® columns.

 

Merck Millipore Application Collection for Chromolith® HighResolution

View a selection of applications with Chromolith® HighResolution and learn how it can support your daily work in the lab.

 

Extraction of Mycophenolic Acid (MPA) and Mycophenolic Acid Glucuronide (MPAG) from Serum Using ISOLUTE® SLE+ prior to LC-MS/MS

This application note describes a simple, efficient and high throughput method for the extraction of the immunosuppressant drug MPA and its metabolite MPAG from fortified serum using ISOLUTE SLE+ in a 96-well plate format.

 

Protein Purification Workflow Development Using Bio-Rad’s NGC™ Chromatography System

High purity protein is a common requirement for biochemical and structural studies. A common approach is to recombinantly express an affinity-tagged version of the protein of interest. This is, however, not always a viable option. Here we discuss protein purification workflow development for untagged proteins and introduce a new indicator of method performance, the purity quotient difference (PQD).

 

Extraction of Antiepileptic Drugs from Serum and Urine using ISOLUTE® SLE+ Prior to LC-MS/MS Analysis

This application note describes the extraction of neutral and zwitterionic antiepileptic (AED) drugs from serum and urine using ISOLUTE SLE+ in a 96-well plate format. The method demonstrates a quick, simple and clean analysis with high levels of recovery achieved.  Using a 96-well plate format facilitates a high throughput work flow model.

 

Molecular Weight Cut-off Determination for Polysulfone Membranes

This application note provides a cost-efficient method for membrane characterization that is robust and fast and can be easily established also in regulated laboratories needing to comply with GxP or FDA 21CFR11.

 

Virtually Particle-Free Rt®-Silica BOND Columns Provide Reliable PLOT Column Performance With Less Time Lost for Maintenance

This application note demonstrates the robustness of the Rt®-Silica BOND column and its performance for many of the applications relevant to testing natural gas and light hydrocarbon streams.

 

The Characterization of Perfume Fragrances Using GC/MS, Headspace Trap and Olfactory Port

This application note reports the results of multiple fragrance analyses using PerkinElmer’s TurboMatrix™ headspace trap coupled with a Clarus® GC/MS and the new GC SNFR™ Olfactory Port. 

 

Aroma Study of Potable Spirits

This application note details the workflow and results of charactering the aroma of potable spirits using the PerkinElmer TurboMatrix™ headspace trap coupled with a Clarus® GC/MS and the new GC SNFR™ Olfactory Port.

 

Characterization of Hop Aroma Using GC/MS, Headspace Trap and Olfactory Port

In this application note the new GC SNFR Olfactory Port is integrated with the Clarus GC/MS to provide a complete aroma profile of hops, capturing human sensory evaluation that is correlated to analytical data.

 

Evaluation of PDMS-Based Extraction Techniques and GC-TOFMS for the Analysis of Off-flavor Chemicals in Beer

Various techniques employing polydimethylsiloxane (PDMS) as an extraction medium prior to GC-TOFMS analysis were investigated to measure off-flavours in aged beer.

 

Fragrance Profiling of Consumer Products using a Fully Automated Dynamic Headspace System

Accurate qualitative and quantitative analysis of perfumed or flavoured products is essential to the flavour and fragrance industry. Especially when unknown samples need to be analysed traditional methods of GC analysis often lead to only vague results and often require time consuming and cumbersome sample preparation techniques such as solvent extraction (liquid/liquid, Soxhlet, Likens-Nickerson).
 

Automated Static and Dynamic Headspace Analysis with GC-MS for Determination of Abundant and Trace Flavour Compounds in Alcoholic Beverages Containing Dry Extract

Direct injection for gas chromatographic profi ling of alcoholic beverages is usually preferable, but where spirits and liquors contain appreciable amounts of non-volatile material, some mode of pre-treatment may be required to avoid both inlet and column contamination.

 

Qualitative Analysis of a Finished Personal Care Product using the GERSTEL MultiPurpose Sampler MPS configured with Multiple Sample Introduction Techniques

This study shows the analysis of a commercially available personal care product using the GERSTEL MultiPurpose Sampler (MPS) configured with Thermal Desorption Unit (TDU), Cooled Injection System (CIS) PTV-type inlet, Dynamic Headspace (DHS) and pyrolysis (PYRO) modules in combination with a GC/MS system. 

 

Qualitative Analysis of Coconut Water Products using Stir Bar Sorptive Extraction Combined with Thermal Desorption-GC/MS

This study shows the analysis of several commercially available coconut water products using a GC/MS system equipped with a versatile autosampler and sample preparation robot capable of performing a wide range of standard sample introduction techniques including thermal desorption. 

 

Flavour and Fragrance Analysis of Consumer Products - Dynamic Headspace Compared to Some Traditional Analysis Approaches

The ability to perform accurate qualitative and quantitative  analysis of perfumes or flavoured products is essential to the  flavour and fragrance industry. Especially when unknown  samples need to be analysed, traditional methods of GC  analysis often lead to only qualitative results and often rely  on time consuming and cumbersome sample preparation  techniques such as solvent extraction (liquid/liquid, Soxhlet,  Likens-Nickerson).

 

Solid-Phase Micro-Extraction (SPME) Coupled with Selectable 1D/2D GC-MS for the Determination of Food Product Flavours

Identification of important trace components in complex  samples like fragrances, natural products, polymers or  food products can be challenging. Achieving the mass on  column and resolution necessary to locate peaks and identify trace components using a single column chromatographic separation can be difficult, if not impossible.
 

Molar Mass Measurements of an Isocyanate Modified Polyurethane Prepolymer in Less than 1 Hour with the EcoSEC GPC System

Isocyanates are both highly reactive and highly toxic low molar mass chemicals. One common technique used to take advantage of isocyanate reactivity while eliminating safety concerns is to synthesize polyurethane prepolymers for use in subsequent polymerizations.

 

Synthesis Monitoring and Oligomeric Analysis of PEGylated Polymers

The utility of SEC for synthesis monitoring and oligomeric analysis makes it an invaluable tool for characterizing synthetic polymeric material for use in medicine, as these materials require thorough characterization amongst other validations.

 

An Approach to Failure Analysis of PC/ABS Resins Used in Automobile Parts: Molar Mass Determination via Gel Permeation Chromatography

The difference between a successful and unsuccessful polymer based material can be determined by observing the molar mass and molar mass distribution of the polymer(s) encompassing the end-use material.

 

InertSustain Phenyl

InertSustain Phenyl is an ideal choise when separation cannot be achieved by hydrophobic interactions provided by C18 or C8 columns.

 

Investigation of the performance of sorptive extraction cartridges for air monitoring

It is demonstrated that despite the considerable advantages of sorptive extraction cartridges for sampling of semi-volatile analytes from liquids, they perform poorly for the higher-volatility analytes that are typically of interest in air monitoring and material emissions applications.

 

Using the CIA Advantage for automated cryogen-free analysis of canister air and gas

Canisters are one of a suite of air sampling technologies for VOCs that are subsequently focused and analysed using thermal desorption with GC(MS).

 

Analysis of a betel-nut foodstuff by direct thermal desorption

The food industry is becoming increasingly aware of the need to detect low-concentration compounds in complex matrices for both product safety and quality.

 

PEGylated Protein Analysis by Size-Exclusion and Reversed-Phase UPLC

PEGylated proteins can be separated by a number of different methods including ion-exchange, size-exclusion and reversed-phase chromatography. For this application, the separation of three species, a 50 KDa molecular weight protein, a 40 KDa activated-PEG and the conjugate, were evaluated using UPLC configurations of both SEC (SE-UPLC) and RPC (RP-UPLC), as these methods can be readily developed to be compatible with an evaporative light scattering detector.

 

Determination of Semivolatile Organic Compounds in Drinking Water Using the Agilent 5977A Series GC-MSD

A method has been developed on the Agilent 5977A Series GC/MSD for the detection of 30 SVOCs at levels as low as 5 parts per billion (ppb), with excellent linearity (R2 > 0.990) and reproducibility (most relative standard deviations (RSDs) ~3.1%). 

 

Development of an Exact Mass LC-MS-MS Library for Screening and Quantitation of Pesticides

An ICP-MS-assisted metallomic approach was used to separatezinc species present in post phloem of Pisum sativum. The use of capillary chromatography was essential due to the low amount of plant sap available. Two zinc species were successfully identified.

 

Quantitation of Trace Level Emerging Contaminants in Water Using Online SPE with LC-MS-MS

A method is developed using the Agilent Infinity Series Online SPE Solution in combination with Triple Quadrupole LC/MS for the analysis of chemicals on US EPA’s Contaminant Candidate List 3 at trace levels in water, with a LOQ < 0.1 for all target compounds. 

 

Rugged GC-MS-MS Pesticide Residue Analysis Fulfilling the USDA Pesticide Data Program (PDP) Requirements

A GC/MS/MS method for the analysis of pesticide residues in fruits and vegetables was developed, optimized, and successfully implemented for routine use in a PDP laboratory. Over 70 pesticides were analyzed in a 20-minute run with excellent method performance.

 

Use of High Resolution “All Ions MS-MS” Mass Spectrometry for Rapid Pesticide Confirmatory Screening

Use a new technique, “All Ions MS/MS”, to rapidly screen, quantify and identify pesticides in food matrices. The analytical method uses a high resolution mass spectrometer to quickly and easily analyze samples and generate quantitative information for target compounds.

 

Sensitive Detection of Pyrethroids in Surface Water and Sediment

A method has been developed on the Agilent 7000 series Triple Quadrupole GC/MS using NCI GC/MS/MS with backflushing. It delivers estimated method detection limits for pyrethroids at 0.05 ppt in water samples and 0.02 ppb for sediment.

 

Speciation of zinc in microliter volumes of plant sap by capillary HPLC-ICP-MS

An ICP-MS-assisted metallomic approach was used to separatezinc species present in post-phloem of Pisum sativum. The use of capillary chromatography was essential due to the low amount of plant sap available. Two zinc species were successfully identified.

 

On-line isotope dilution analysis with the 7700 Series ICP-MS: Analysis of trace elements in high matrix samples

This work describes a simple, accurate and precise ICP-MS method for the direct determination of trace elements in high matrix samples by on-line isotope dilution analysis. The effective dynamic range for the method is more than 4 orders of magnitude (0.1 to 1000 μg/L). 

 

InertSustain Full Catalogue - from GL Sciences

InertSustain employs a radically new type of silica, in which the surface of the silica is uniquely modified, enabling precise control of the silica properties.

 

InertSustain C8

InertSustain C8 is an octyl group (C8) bonded column delivering the same extreme inertness to any type of compounds just like InertSustain C18, which enables rapid analysis of highly hydrophobic compounds delivering symmetric peaks at a wide range of pH.

 

InertSustain NH2

Inertsil NH2 is another Phenylpropyl bonded column from GL Sciences. By employing the new Silica gel, InertSustain NH2 is more durable than Inertsil NH2.

 

InertSustain C18

Highly end-capped ODS column such as InertSustain C18 offers an opportunity to flush out contaminants from the column surface easily using an organic solvent.

 

Autom. Measurement of Conductivity, pH and Turbidity in Potable Water (Part 2)

In this method the fully automated measurement of conductivity, pH and turbidity of potable water samples is presented.

 

Autom. Measurement of Conductivity, pH and Turbidity in Potable Water (Part 1)

In this method the fully automated measurement of conductivity, pH and turbidity of potable water samples is presented.

 

Chemical Oxygen Demand (COD) of Waste Water: Sample Titration

Determination of the COD value in waste water according to DIN 38409 part 4, H4. This application describes the sample titration. For back value determination check application M438-2, whereas for automated sample preparation see M438-1.

 

Chemical Oxygen Demand (COD) of Waste Water: Back Value Determ

Determination of the COD value in waste water according to DIN 38409 part 4, H4. This application describes the determination of the back value for titration. For sample titration check application M438-3, whereas for automated sample preparation see M438-1.

 

Chemical Oxygen Demand (COD) of Waste Water: Sample Preparation

Determination of the COD value in waste water according to DIN 38409 part 4, H4. This application describes the automated sample preparation using the Rondo 60 sample changer. For sample titration check application M438-3, whereas for COD back value determination see M438-2.

 

UC17 article - Double throughput and double efficiency through clever lab automation

Chloride determination is performed as an indicator for correct flavor dosage in snacks manufacturing at PepsiCo Frito-Lay’s Snack Food site in Belgium. A new approach in automated titration was necessary in order to increase sample throughput in quality control. Parallel execution of two bottleneck steps could double this throughput. At the core of the new process is a titrator, a sample changer (in double tower configuration) and a temperature control device.

 

UC15 article - The modern and efficient approach to routine tasks in water analysis

Alkalinity, pH, conductivity and turbidity are some of the parameters routinely measured every day in water laboratories. These parameters are usually determined using standalone instruments and time-consuming procedures that do not always ensure the necessary traceability of the results. Other analytical procedures such as COD determination are also lengthy and involve the use of aggressive chemicals, with a potential health hazard for the operator. METTLER TOLEDO offers specific and flexible solutions to fully automate these analyses.

 

The Ultimate Salt Guide

Salt and humans go a long way together. In earlier times, before mining of rock salt had started, salt was a high-priced and much sought after commodity. Nowadays, with cheaper salt prices, salt is a key ingredient in processed foods. This guide will:
    • Give insights into methods of salt determination in food
    • Provide a short overview of the history of salt
    • Show and explain measurement in selected samples
    • Present a few tips and hints to improve operator technique on titrators and balances.
 

Acid and Chloride Content in Wine

Method for the determination of tartaric acid and chloride in wine. The analysis is monitored with a pH glass combined electrode as well as a combined silver ring electrode.

 

Sample Preparation for Karl Fischer Titration Guide 2

The Karl Fischer method determines water content specifically and is easily applied to a huge variety of samples. It is a common standard method in R&D, quality control and production monitoring. However, the method requires adepuate sample preparation in order to release entrapped, capillary-bound or water of crystallization. The water molecules need to be 'freely available' in order to undergo the chemical reaction with the KF reagents. This brochure uses METTLER TOLEDO's expert knowledge of Karl Fischer titration to explain more advanced sample preparation procedures than the simple sample dissolution in the titration cell.

 

The correct and comprehensive calculation of the measurement uncertainty of analytical

procedures represents one of the greatest challenges of laboratories accredited to ISO/IEC/EC/DIN 17025 (2005). A previous article introduced the basic principles, whereas further aspects are presented here using a concrete example from daily titration practice.

 

UC16 Article - Measurement uncertainty in daily practice

The correct and comprehensive calculation of the measurement uncertainty of analytical procedures represents one of the greatest challenges of laboratories accredited to ISO/IEC/EC/DIN 17025 (2005). A previous article introduced the basic principles, whereas further aspects are presented here using a concrete example from daily titration practice.

 

Extraction of Synthetic Cannabinoids (SPICE) from Oral Fluid Using ISOLUTE® SLE+ 96-well Plates and Columns Prior to LC-MS/MS

This application note describes the extraction of a range of SPICE drugs and metabolites from neat oral fluid and oral fluid from a commercial collection kit using ISOLUTE® SLE+ in both 96-well plate and column formats.

 

Analyzing Residual Solvents in Pharmaceutical Products Using GC Headspace with Valve-and-Loop Sampling

Residual solvents were detected by following the USP 467 method using a new valve and loop autosampler configured with a solid, fully integrated, and reliable platform with full auditing capability.

 

Simplifying Complex Multi-Residue Pesticide Methodology in GC-MS/MS

Ease the implementation and management of multi-residue pesticide methodologies with a system configuration that includes a complete instrument method with compound retention times and MRM parameters already included —eliminating days, if not weeks, of method development.

 

Moving from Helium to Hydrogen as a Carrier Gas for the Thermo Scientific ISQ GC-MS System

Using hydrogen as a carrier gas for GC-MS rather than the traditional use of helium, this method demonstrates an economical and reliable use of a hydrogen generator for a safe, steady, and renewable supply of hydrogen.

 

Determination of Polychlorinated Dibenzo-p-dioxins and Furans (PCDD/Fs) in Routine Environmental Samples

Using especially sensitive triple-quadrupole GC-MS/MS systems that perform at HRMS sensitivity levels, this environmental analysis method incorporates data-processing software designed to handle complex calculations associated with dioxins analysis.

 

Rapid, Automated, and Accurate Determination of Volatiles in Human Blood by Headspace Gas Chromatography

Blood alcohol levels were determined using a dual-column configuration to provide automated and reproducible results with excellent throughput and auditing capabilities convenient for a regulated environment.

 

High Sensitivity Analysis of Nitrosamines Using GC-MS/MS

Analyze nitrosamines in beer using a simple and standard approach that utilizes the regular electron impact ionization (EI) and AutoSRM software for a very straightforward MRM method for low-level nitrosamine analysis.

 

Broad Scope Pesticide Screening in Food Using Triple Quadrupole GC-MS

Smart instrument control and data processing software are applied to the GC-MS/MS analysis of 600 pesticides in matrix to mitigate analytical performance degradation through the MS duty cycle.

 

Detection, Identification, and Quantitation of Azo Dyes in Leather and Textiles by GC/MS

Analyze azo dyes in cotton and silk textiles using this method that is compliant with the EN ISO 14362-1 standard procedure and eliminate false positive peaks with a data processing method that performs QA/QC and confirming ion checks.

 

Distilled Spirit Analysis using the New 100 % Aqueous Stable Zebron™ ZB-WAXplus

WAX columns provide optimal selectivity for many aqueous soluble compounds such as those found in alcoholic beverages. Historically, polyethylene glycol (PEG) phases have been unstable with aqueous samples resulting in poor reproducibility and decreased lifetime. The new Zebron ZB-WAXplus bonding procedure results in exceptional stability to repeated injections of aqueous matrices.

 

Analysis of Organophosphorus Pesticides in Baby Foods Using a Triple-Quadrupole GC/MS/MS System

Contamination of food products with pesticides is a growing concern because of recognized adverse health effects, increasing world-wide usage of pesticides, and increasing imports of raw foodstuffs from foreign sources. The concern is particularly acute for baby foods because of the high vulnerability of babies to adverse health effects from synthetic chemicals, particularly pesticides.

 

Trace Oxygenated Hydrocarbons in Liquid Hydrocarbon Streams by Multidimensional GC

It has been widely accepted that oxygenates are related to corrosion and fouling issues in refinery processes. Accurate determination of trace oxygenated hydrocarbons in liquid hydrocarbon streams plays an important role in process design and operation. Method UOP 960 defines testing procedures utilizing a valved gas chromatograph (GC) system. A non-polar column accumulates components of interest, and a polar column is used to separate oxygenates. In fact, the  instrumentation is a prototype of multidimensional GC (MDGC) that requires complicated setup and configuration. Determination of valve timing, however, has been proven to be a daunting task. Operators work at optimizing parameters in a trialand- error process, which is both laborious and time consuming.

 

Methods 8260C and 8270D on a Single GCMS without Changing Columns

USEPA Methods 8260C (volatile) and 8270D (semi-volatile) typically require dissimilar chromatographic columns with incompatible maximum temperatures. Historically, laboratories performing these analyses have found it necessary to allocate separate GCMS instrumentation for the two analysis modes, or perform frequent reconfiguration (column changing) to run these methods on a single GCMS unit. Breaking the MS vacuum to change analytical columns is time-consuming and inefficient, however productivity can be improved significantly using the Shimadzu Twin Line MS Kit. With this configuration, the user can easily switch between applications without breaking vacuum to change the analytical column.

 

Simultaneous Analysis of Evolved Gas Produced by the Degradation of a Lithium-Ion Battery

In evaluating the degradation of lithium-ion rechargeable batteries, it is necessary to analyze the gases produced inside the battery. The composition of the sampled internal gases can be investigated by conveying them to a gas chromatograph. 

 

High-Sensitivity Simultaneous Analysis of Inorganic Gases and Light Hydrocarbons

With conventional analytic methods, the high-sensitivity detection of CO, CO2 and light hydrocarbons requires a Methanizer plus a flame ionization detector (FID), while the detection of inorganic gas components requires a thermal conductivity detector (TCD). This requires a system with a complicated flow channel configuration.

 

Analysis of Reaction Products in Artificial Photosynthesis Research

Artificial photosynthesis refers to a technique for the manufacture of high-energy substances using energy from sunlight. It is expected to become the 4th type of sunlight-based renewable energy after solar cells, solar heating, and biomass technologies.

 

Environmental Volatiles Using an Agilent 7697A Headspace Sampler, an Agilent 7890b gc, and an Agilent 5977A Series GC/MSD

The Agilent 7697A Headspace Sampler, AGILENT 7890b gc, AND aGILENT 5977A Series GC/MSD system with extractor lens was used for the headspace analysis of environmental volatiles in water. EC reporting requirements, as outlined in the 98/83/EC Directive update July 2009, were met for all compounds. Calibration was from 0.05 parts-per-billion (ppb)-20 ppb with excellent linearity. Peak shapes were very good for all compounds including the early eluting gases.

 

Applying the Agilent 5977A MSD to the Analysis of USP,467> Residual Solvents with the 7697A Headspace Sampler and 7890B GC

The Agilent 7697A Headspace Sampler coupled to an Agilent 5977 Series GC/MSD System was used for the analysis of USPresidual solvents at their limit concentration in aqueos solution according to procedure A of the method.

 

Agilent Inert Flow Path Enhancements Improve Drugs of Abuse Testing

An evaluation of Siltite versus Agilent UltiMetal Plus Flexible Metal ferrules installed in an Agilent Ultimate Union showed improved benzodiazepine peak shape and response for UltiMetal Plus Flexible Metal ferrules by FID.

 

Analysis of USP 467 Residual Solvents using the Agilent 7697A Headspace Sampler with the Agilent 7890B Gas Chromatographer

USPresidual solvents were analyzed by static headspace on the Agilent 7697A Headspace Sampler combined with the Agilent 7890B Gas Chromatograph. The previously descrived method performed on an Agilent 7890A GC was directly transferred to the 7890B GC. Excellent chromatographic performance was acheived at USPspecified limits and equivalent results were obtained. This test clearly indicated that methods can be transferred directly from an Agilent 7890A GC to the 7890B GC without modification.

 

Improved Inertness and QC Testing Standards for EPA Method 8270D with Zebron™ ZB-SemiVolatiles GC Columns

Increased column activity can lead to poor acid/base sensitivity and analyte misidentification, which are common hindrances to the accuracy of semi-volatile methods. This is most apparent when analyzing compound lists with various types of functional groups and reactivity characteristics, as in EPA Method 8270. This study explores the inertness of leading GC columns used for semivolatiles methods and presents the advantages afforded by using columns designed and QC tested specifically for EPA 8270D.

 

Improved High Temperature Simulated Distillation (ASTM D6352 and D7169) Using Zebron™ ZB-1XT SimDist Metal GC Columns

An improved method for high temperature simulated distillation based upon ASTM D7169 is presented using the Zebron ZB-1XT SimDist column. This column utilizes a Glass Infusion™ Technology that results in more improved efficiency, resolution, and unmatched column-to-column reproducibility. This technology also allows simulated distillation methods, such as ASTM D6352 and D7169, to be extended from C100 to C120 while still meeting all the system suitability requirements.

 

Analysis of Human IgG Glycans on a Solid Core Amide HILIC Stationary Phase

This application note demonstrates the analysis of human IgG glycans labeled with a fluorescent tag (2-aminobenzamide) by hydrophilic interaction liquid chromatography (HILIC). The separation is carried out with a Thermo Scientific™Accucore™150-Amide-HILIC 150 Å pore diameter solid core HPLC column. The method displays excellent separation at backpressures compatible with conventional HPLC systems.

 

Separation of 2AB Labeled N-Glycans from Bovine Fetuin on a Novel Mixed-Mode Stationary Phase

This application note demonstrates the analysis of fluorescently labeled N-glycans released from proteins (bovine fetuin) and separated by hydrophilic interaction liquid chromatography (HILIC) / weak anion exchange mixed-mode chromatography. The separation is carried out with a 1.9 μm Thermo Scientific™ GlycanPac™ AXH-1 column using fluorescence detection. The method exhibits excellent separation based on charge, size, and polarity. This phase also provides a unique tool for quantifying glycans based on charge.

 

Structural Analysis of Labeled N-Glycans from Proteins by LC-MS/MS Separated Using a Novel Mixed-Mode Stationary Phase

This application note describes the liquid chromatography-mass spectrometry (LC/MS) analysis of fluorescently labeled N -glycans released from proteins. The chromatographic separation is carried out with a novel Thermo Scientific™ GlycanPac™ AXH-1 (1.9 μm, 2.1 × 150 mm) column for high-resolution and high-throughput analysis of glycans. This column possesses unique selectivity that provides separation of glycans based on charge, size, and polarity. MS and MS/MS analyses are performed using a Thermo Scientific™ Q Exactive™ hybrid quadrupole-Orbitrap™ mass spectrometer in negative ion mode to provide detailed structural information of N -glycans released from proteins.

 

A Novel Affinity Protein A Column for Monoclonal Antibody (MAb) Titer Analysis

The Thermo Scientific™ MAbPac™ Protein A column is a high-performance affinity chromatography column specifically designed for the determination of monoclonal antibody concentration in harvest cell culture. The nonporous, hydrophilic stationary phase enables fast and accurate MAb titer analysis. The ability to collect the IgG fraction during the HPLC analysis allows the analyst to characterize the IgG charge variants using a novel pH gradient approach.

 

A Novel pH Gradient Separation Platform for Monoclonal Antibody (MAb) Charge Variant Analysis

MAb charge variants and protein standards with various pI values have been successfully separated using cation exchange chromatography with a linear pH gradient. This linear pH gradient is generated by running a linear pump gradient from 100% buffer A (at pH 5.6) to 100% buffer B (at pH 10.2). Ruggedness testing of this pH gradient on Thermo Scientific™ MAbPac™ SCX-10 columns shows that retention time RSD is less than 0.8% over 300 runs.

 

Fast, Quantitative SPE LC-MS/MS Analysis of Montelukast in Human Plasma

A fast HPLC method and an efficient extraction and analysis method for montelukast in human plasma has been developed using a Thermo Scientific™ SOLA™ SAX SPE 96 well plate and a Thermo Scientific™ Accucore™ C8 HPLC column. The sample preparation was fast, reproducible, and accurate. The chromatographic method provides analysis time of less than 1.5 minutes. The dynamic range was linear between 1 and 1000 ng/mL with an R2 of 0.9901.

 

Mixed-Mode, Weak Anion-Exchange, Solid-Phase Extraction Method for the Extraction of Niflumic Acid from Human Plasma

An HPLC-MS/MS method has been developed for the determination of niflumic acid in human plasma. This application note demonstrates the use of Thermo Scientific™ SOLA™ WAX SPE products, which allow mixedmode extractions to be carried out with strong acids, giving improved removal of matrix interferences and reproducible results. The use of a Thermo Scientific™ Accucore™ HPLC column provided fast and efficient separation without the need for an ultra high pressure system. MS/MS detection was performed on a Thermo Scientific™ TSQ Vantage™ mass spectrometer.

 

LC-MS/MS Analysis of Edrophonium, Neostigmine, and Pyridostigmine in Plasma Using HILIC Chromatography and Weak Cation-Exchange SPE

A liquid chromatography-tandem mass spectrometry method for the analysis of edrophonium, neostigmine, and pyridostigmine in plasma has been developed. Analysis was carried out using Thermo Scientific™ SOLA™ WCX solid phase extraction (SPE) products, a Thermo Scientific™ Syncronis™ hydrophilic interaction liquid chromatography (HILIC) UHPLC column for separation, and a Thermo Scientific™ TSQ Vantage™ mass spectrometer for MS/MS detection.

 

HPLC-UV Method for the Determination of Asenapine Maleate Impurities Using a Solid Core C8 Column

Asenapine maleate is a novel drug recently approved by the United States Food and Drug Administration for treatment of acute schizophrenia and for manic or mixed episodes of bipolar I disorder, with or without psychotic features, in adults. This application note demonstrates a simple and rapid method for the determination of asenapine maleate impurities using a Thermo Scientific™ Accucore™ C8 HPLC column.

 

High-performance screening of pollutants in water using GC×GC/TOF MS

This Application Note demonstrates how the latest sampling techniques, combined with GC×GC separation and BenchTOF-dx detection, offer considerable advantages for the identification of pollutants in river water. The quality of the analysis is illustrated by reference to the detection of PAHs, PCBs and pesticides, while the ability of the method to detect ‘unknowns’ with little additional effort is demonstrated by the identification of polycyclic musks.

 

Time-of-flight mass spectrometry applied to the identification and quantitation of trace-level compounds in beer

This Application Note shows that BenchTOF-dx is a powerful detector for the trace-level flavour compounds present in the complex profiles resulting from the sorptive extraction of beer. The generation of linear responses at sub-ppb levels is a particular feature of the work, while the ability of BenchTOF-dx to produce ‘classical’ spectra matching those in commercial libraries greatly simplifies automated compound identification.

 

Analysis of polycyclic aromatic hydrocarbons from vehicle exhaust using TD–GC/TOF MS

This Application Note describes the use of BenchTOF-dx and TargetView to confidently identify polycyclic aromatic hydrocarbons (PAHs) in diesel exhaust particulate. The sensitivity and ‘classical’ spectra produced by BenchTOF-dx allow accurate identification of PAHs with near-identical fragmentation patterns, while TargetView enables GC profiles of trace-level analytes to be visualised even when hidden under much more abundant components.
 

BenchTOF-dx and TargetView – High-definition, versatile technologies for the identification of TO-15/TO-17 ‘air toxics’

This Application Note demonstrates the use of the BenchTOF-dx and TargetView for testing ambient air for ‘air toxics’ using US EPA methods TO-15 and TO-17. We demonstrate that the mass sensitivity and ‘reference-quality’ spectra of BenchTOF-dx, combined with the library-matching capability of TargetView, allow the confident identification of compounds over a range of concentrations, exemplified in this case by styrene (≈1 ppb) and trichloroethene (≈20 ppt).

 

Enhanced identification of drugs of abuse in urine using time-of-flight mass spectrometry

This Application Note describes the use of BenchTOF-dx to detect drugs of abuse in urine using fast GC. The application demonstrates the high sensitivity of BenchTOF-dx, its production of ‘reference-quality’ mass spectra, as well as its ability to handle narrow peaks produced by fast GC. Of particular note is the detection of benzodiazepines, which have been historically difficult to detect by GC/MS due to their polarity.

 

Fingerprinting of crude oil by GC×GC/TOF MS

This Application Note shows that BenchTOF-dx can be successfully used as the detector for the GC×GC analysis of a crude oil distillate. By focusing on the trace-level chemicals needed for oil characterisation, it is demonstrated that the combination of ‘reference-quality’ spectra and high sampling frequency make BenchTOF-dx ideal for this challenging application.

 

Application of TargetView software in the food industry – The identification of pyrazines in potato crisps

This Application Note describes the use of TargetView to automate the detection of important flavour compounds in complex aroma profiles. Processing of the GC/MS chromatogram resulting from headspace sampling of potato crisps allowed detection of three trace-level pyrazines, even though they were hidden under a complex background.
 

An Alternative USP Method for the Analysis of Impurities in Riboflavin (Vitamin B2) Using LC-MS/MS

Riboflavin (vitamin B2) is a water-soluble vitamin. It is synthesized by all plants and many microorganisms, but it is not produced by higher animals. It is a precursor of coenzymes that are required for the enzymatic oxidation of carbohydrates, so it is essential to basic metabolism.

 

Introducing Titan UHPLC Columns: Setting a New Performance Standard

Evidence shows that superior HPLC and UHPLC column performance for solid-core and other columns correlates well with a tighter particle distribution and lower A-term (eddy diffusion) in the van Deemter equation.

 

Determination of Additives in Beverages Using Ascentis® Express Columns

Beverages, such as sodas and energy drinks, can include a number of polar ingredients, which are easily soluble in the water matrix of the drinks. These ingredients include sweeteners (sugars and sugar substitutes), caffeine, vitamin supplements, amino acids, organic acids, and plant extracts.

 

Impact of Instrument Dispersion on Performance of HPLC Capillary Columns

The HPLC system flow path comprises column plus instrument components that include valves, tubing, and detector(s). Band spreading occurs as the sample traverses through each component.

 

A Novel Approach in HPLC Chiral Method Development: Dealing with Multiple Chiral Centers

Development of methods capable of robust and reproducible separation of enantiomers is significantly challenging. Many traditional pharmaceutical compounds exhibit multiple chiral centers, requiring methods that can at least separate the potential enantiomers and diastereomers from the API. Even more desirable is a method that can separate each of the potential isomeric impurities for accurate quantitation.

 

Rapid Cleanup of Spinach Extracts Using Gravity Elution SPE Prior to Pesticide Analysis

Prior to analysis for pesticide residues, extracts of highly pigmented foods, such as spinach, require a cleanup step for removal of matrix materials. Failure to do so can lead to ion suppression in LC-MS, inlet contamination in GC-MS and column contamination for both techniques. A dual-layer SPE tube containing graphitized carbon and aminopropyl on silica (NH2) is often used.

 

Fundamental Investigation Regarding Robustness and Repeatability in HILIC Chromatography

Interest in chromatography using hydrophilic interaction liquid chromatography (HILIC) has continued to build in recent years. In this mode of chromatography, analyte retention increases monotonically with an increase in the organic component of the mobile phase.

 

The Extraction of Glycols From Water Using ENVI-Carb Plus Solid Phase Extraction Cartridges

Glycols and glycol ether compounds are used in a wide variety of applications, including de-icing solutions and toxic chemical dispersants. The oil spill in the Gulf of Mexico in 2010 resulted in the widespread use of Corexit™ 9500 dispersant, which contains propylene glycol. The analysis of glycols such as propylene and ethylene glycol from water samples is traditionally done by direct aqueous injection (DAI) into a gas chromatograph. Aqueous injections are problematic in GC analysis due to issues such as the large expansion volume of water in the inlet, increased carryover, and elevated detection limits.

 

Sampling Technique for Qualitative Volatile Headspace Outgassing from Solid Matrices

Volatile compounds in solids have always presented a challenge for the chromatographer. The common approach of testing by static headspace is limited by the compound concentration and sample volume. Selective solvent extraction is another common sample preparation technique.

 

Automated Determination of Total Fat, Saturated Fat, Monounsaturated Fat and Trans Fat Content in Food Samples

Determination of total fat, saturated fat, monounsaturated fat and trans fat content in food samples is necessary for complying with applicable food labeling requirements. A typical procedure for saponifi cation of the sample involves refl uxing with sodium methoxide in methanol, followed by a second reflux with boron trifluoride in order to esterify the free fatty acids. Prior to injection into the gas chromatograph, the fatty acid methylesters (FAMEs) must be extracted from the reaction mix and the extract must be dried. The reflux times are typically an hour. After the sample is prepared, the round bottomed flask and condenser must be cleaned. This process is laborious and time consuming, which limits sample throughput.

 

Analysis of 19 EPA Polychlorinated Biphenyls by GC/MS using Hydrogen Carrier Gas

For many GC applications, hydrogen is the carrier gas of choice, due to its superior qualities in terms of analysis speed and increased response. However, its use in GC/MS has widely been avoided due to concerns over safety, high background noise, and potential reactions in the ion source.

 

TSKgel SuperSW mAb HTPHR

Aqueous size exclusion chromatography (SEC) is the method of choice for the analysis of protein fragments, monomers, and aggregates under non-denaturing conditions. Based on the flow of the sample through a porous stationary phase SEC separates molecules according to their size, or more precisely, their hydrodynamic volume.

 

High Speed and Resolution SEC Analysis of mAbs Using TSKgel SuperSW mAb Columns

Antibody therapeutics are enjoying high growth rates in the biopharmaceutical market, the major areas of therapeutic application being cancer and immune/inflammation-related disorders including arthritis and multiple sclerosis. In 2010, four of the top ten best-selling global drug brands were monoclonal antibodies (mAbs).

 

Microbial Quality Control of Beer

The classic microbiological methods used in the quality control of beer are still important. Conventional, standard-based cultivation methods are very time consuming and take 3 to 5 days for results. Most modern methods use at least a pre-enrichment step with minimal cost for the analysis and mak

 

Rapid and sensitive aroma profiling of strawberries using dynamic headspace sampling and TD–GC/TOF MS

This Application Note describes the fast and highly sensitive detection of trace-level aroma compounds in the headspace gas above fresh strawberries.

 

Increasing Peak Capacity in Reversed-Phase Peptide Separations with Charged Surface Hybrid (CSH) c18 Columns

Peptide separations are of paramount importance, whether studying proteins by bottom-up proteomics or thoroughly characterizing biopharmaceuticals using peptide mapping. The mixtures encountered in these analyses are inherently complex. Reversed-phase (RP) chromatography has become the separation mode of choice, as it offers relatively high resolving power and easily interfaces with mass spectrometry (MS).

 

UPLC/MS/MS Determination of Aminoglycoside Antibiotics in Meat and Milk

Aminoglycoside Antibiotics, used in veterinary medicine for the treatment of animals bred for meat and milk production, require an effective method for residue analysis in these commodities. This class of antibiotic presents significant challenges for residue analysis. Unlike most other antibiotic classes, these compounds are not amenable to extraction from tissue or milk using acetonitrile or other solvents. In this study, the aminoglycosides are extracted from meat tissue or milk using an aqueous buffer with trichloroacetic acid (TCA) added to percipitate protein and inhibit protein binding of the analytes.

 

Improving Performance and Throughput of the USP Organic Impurities Analysis of Tioconazole on an Alliance HPLC System

Organic impurities in generic drugs are routinely analyzed by pharmaceutical manufacturers worldwide. Performing organic impurities analysis with older instruments and column technology can be time-consuming and costly, as these methods can be very lengthy and require large amounts of solvent. However, by using more modern chromatographic tools, organic impurities assays can become more efficient due to significant improvements in both instrumentation and column technology.

 

Development of a Quantitative SPE-LC/MS/MS Assay for Teriparatide in Human Plasma

Teriparatide (FORTEO) is a recombinant form of a fragment of human parathyroid hormone, used in the treatment of osteoporosis. As a major global health problem, osteoporosis is responsible for 1.5 million bone fractures each year/ Teriparatide is the first treatment for osteoporosis that actually stimulates new bone formation. It is an anabolic drug that acts to strengthens bones wit the potential to improve skeletal micro architecture, thereby increasing bone density. In contract to biosphosphonate drugs that treat osteoporosis by reducing or preventing bone loss, teriparatide promotes bone production.

 

Direct Analysis of Urinary Opioids and Metabolites by Mixed-Mode µElution SPE Combined with UPLC/MS/MS for Forensic Toxicology

The analysis of natural and synthetic opioid drugs continues to be an important aspect of forensic toxicology. In the past, analyses were typically conducted by GC/MS after first subjecting the samples to acid or enzymatic hydrolysis to liberate glucuronide metabolites. With the advent of LC/MS/MS techniques, glucuronide metabolites can eliminate the risk of false negatives due to incomplete hydrolysis, as enzymatic efficiency can vary greatly depending upon the enzyme used and the drug substrate analyzed.

 

Reproducible Analysis of Monoclonal Antibodies and Proteins

Gel Filtration Chromatography is popular among biochemists for the characterization of proteins and mAbs. TSKgel G3000SWXL columns are the industry’s workhorse for antibody analysis in quality control. This application note reports the analysis of monoclonal antibodies using TSKgel G3000SWXL demonstrating the effectiveness of the proprietary surface chemistry.

 

SEC Analysis of Monoclonal Antibodies

Size exclusion chromatography (SEC) is the standard method for aggregate and fragment analysis of monoclonal antibodies in biopharmaceutical QC. A new series of silica-based SEC columns was engineered to provide shorter analysis time or higher resolution than standard columns for the separation of fragments, monomers, and aggregates.

 

SEC-UV-RI-MALS

Static light scattering in combination with size exclusion chromatography is a valuable tool for verifying purity of monoclonal antibodies (mAbs) as such or as a quick check while the downstream processing takes place. Besides fluorescence detection, light scattering is one of the most sensitive methods to detect protein aggregates.

 

Characterizing Biotherapeutics with HPLC

A thorough characterization of therapeutic biomolecules is a key task for the successful submission of data for regulatory approvals of new drugs. HPLC is frequently used when establishing analysis methods for biologics or biosimilars. This article features some of the most frequently used HPLC applications for the characterization of biopharmaceuticals.

 

HPLC-UV Method for the Determination of Asenapine Maleate Impurities Using a Solid Core C8 Column

Asenapine maleate is a novel drug recently approved by the United States Food and Drug Administration for treatment of acute schizophrenia and for manic or mixed episodes of bipolar I disorder, with or without psychotic features, in adults. This application note demonstrates a simple and rapid method for the determination of asenapine maleate impurities using a Thermo Scientific™ Accucore™ C8 HPLC column.

 

High-Throughput Analysis of Dextromethorphan and Dextrorphan

Dextromethorphan is used as a cough suppressant and can be found in many over-the-counter cough and cold remedies. Dextromethorphan is quickly metabolized to dextrorphan in the liver. This process can be used to assess the speed of metabolism. The retention, peak shape, and resolution of dextromethorphan and dextrorphan are demonstrated in this application , using a Thermo Scientific™  Accucore™ C18 HPLC column.

 

Determination of Gestodene in Human Plasma by SLE-LC-MS/MS Using a Solid Core HPLC Column

A simple, rapid, and sensitive procedure for the determination of gestodene in human plasma by liquid chromatography-tandem mass spectrometry was developed and evaluated. The drug was isolated from a plasma matrix using Thermo Scientific™ HyperSep™ SLE, and the components of the resultant extracts were separated on a Thermo Scientific™ Accucore™ C18 HPLC column under reversed-phase, gradient conditions. Detection was performed on a triple quadrupole mass spectrometer using positive polarity, heated electrospray ionisation (HESI) conditions operating in selected reaction monitoring (SRM) mode.

 

Comparative Analysis of Cooking Oils Using a Solid Core HPLC Column

Cooking oils derive from many sources, each with a characteristic profile of triglycerides. The major components are frequently similar, so it is important to resolve even the minor constituents. The Thermo Scientific™ Accucore™ C30 HPLC column excels at distinguishing among subtly different large hydrophobic molecules. The optimized bonding density of the long alkyl chains facilitated by a wider pore diameter particle results in a phase that is stable even in highly aqueous mobile phases. The Accucore C30 phase offers greater selectivity and resolution of minor components when compared to the C18 phase.

 

LC-MS/MS Method for the Determination of Docetaxel in Human Serum for Clinical Research

A liquid chromatography-tandem mass spectrometry method for the analysis of docetaxel in human serum for clinical research has been developed. Using Thermo Scientific™ SOLA™ cartridges or plates, sample preparation is fast and gives excellent reproducibility and recovery levels. The analysis was carried out on a Thermo Scientific™ Accucore™ RP-MS HPLC column (2.6 μm, 50 x 2.1 mm) for a fast separation with a cycle time of 2 minutes and excellent peak shape.

 

Determination of Pregabalin in Human Plasma by SPE-LC-MS/MS Using Mixed Mode Solid Phase Extraction Cartridges and a Solid Core HPLC Column

A simple, rapid and sensitive procedure for the determination of pregabalin in human plasma by liquid chromatography-tandem mass spectrometry was developed and evaluated. The drug was isolated from a plasma matrix using Thermo Scientific™ SOLA™ CX solid phase extraction material, and the components of the resultant extracts were separated on an Thermo Scientific™ Accucore™ PFP HPLC column under reversed-phase, gradient conditions. Detection was performed on a triple quadrupole mass spectrometer using positive polarity, heated electrospray ionisation (HESI) conditions operating in selected reaction monitoring (SRM) mode.

 

SPE-LC-MS/MS Method for the Determination of Nicotine, Cotinine, and Trans-3-hydroxycotinine in Urine

A liquid chromatography tandem mass spectrometry method for nicotine, cotinine, and trans-3-hydroxycotinine in urine has been developed. Using Thermo Scientific™ SOLA™ CX cartridges or plates, sample preparation is fast, giving excellent reproducibility and recovery levels for each compound. The analysis was carried out on a Thermo Scientific™ Syncronis™ C18 1.7 μm, 50 x 2.1 mm column for a fast separation with a cycle time of 3 minutes while maintaining excellent peak shape.

 

Fast Extraction of Metanephrine and Normetanephrine from Synthetic Urine using EVOLUTE EXPRESS CX in a 96 Fixed Well Plate Prior to LC-ESI-MS/MS

The normalized metabolite concentrations of epinephrine and norepinephrine precursors have common utility in clinical diagnostics related to neuroendocrine tumors. Of particular interest are the selected metabolites metanephrine and normetanephrine.

 

A Comparison of the Extraction of Beta Blockers from Plasma Using Solid-Supported Liquid-Liquid Extraction and Traditional Liquid-Liquid Extraction

Beta blockers (or beta antagonists) are a category of drugs used to treat a number of medical complaints, such as hypertension, angina, heart failure, and heart attacks. Beta blockers are designed to stop the functioning of a naturally occurring compound, noradrenaline. Noradrenaline is a chemical released in the body that can cause the arteries to narrow and the heartbeat to increase.

 

Analysis of Benzoic, p-Toluic, and Terephthalic Acids Using Anion-Exchange HPLC

Terephthalic acid is predominately used as the starting material in the production of polyethylene terephthalate (PET), which is used in the manufacture of clothes, plastic bottles, and inner coatings of food cans.

 

Determination of Melamine in Powdered Milk by LC-MS/MS Using a Core Enhanced Technology Solid Core HPLC Column

In recent years melamine has been found in adulterated milk and milk based products, especially in infant formula milk, causing thousands of children to become ill. Limits have now been set for the amount of melamine that can be present in foodstuffs; for infant formula milk this level is zero and for other food stuffs there is a 2.5 ppm maximum.

 

Fast, Reproducible LC-MS/MS Analysis of Dextromethorphan and Dextrorphan

A liquid chromatography–tandem mass spectrometry method for the analysis of dextromethorphan and dextrorphan from rat plasma has been developed. A limit of quantification of 0.1 ng/mL is readily achieved.

 

LC-MS/MS Method for the Determination of Paclitaxel in Human Serum

A liquid chromatography tandem mass spectrometry method for the analysis of paclitaxel in human serum has been developed. Using Thermo Scientific™ SOLA™ cartridges or plates, sample preparation is fast and reproducible giving excellent recovery levels.

 

LC-MS/MS Method for the Determination of Tenofovir from Plasma

A liquid chromatography-tandem mass spectrometry method for tenofovir from plasma has been developed. Using Thermo Scientific™SOLA™CX plates, sample preparation is fast and efficient, giving excellent recovery levels for the compound.

 

Determination of Zolmitriptan in Serum by SPE-LC-MS/MS

A liquid chromatography-tandem mass spectrometry method for the analysis of zolmitriptan in serum has been developed. A limit of quantitation of 1 ng/mL is readily achieved.

 

The Ultimate Acidity Guide

Acidity of food items is an important topic within the food industry. There are personal
and cultural differences in taste and considerations about storability that make a close
monitoring of acidity in food products necessary.

 

Introduction to Karl Fischer Titration

The Karl Fischer method for the water content determination is one of the most frequently used Titration methods.

 

Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl

Titration Excellence Line: The buffer capacity of the acidic mixture HCl, CH3COOH and NH4Cl and the concentration of each acid was determined by potentiometric titration with the DG112-Pro electrode.

 

Total Hardness of Tap Water by Photometric Titration

The total hardness of water, expressed as CaCO3 content of water is determined by complexometric titration of calcium and magnesium at pH 10 using EDTA. The color change of the Erio T indicator (violet to blue) at the equivalence point is sensed by a DP5 PhototrodeTM.

 

Calibration of a DX219-F Fluoride Ion Selective Electrode

Titration Excellence Line: Method for the adjustment (calibration) of the DX219-F fluoride ion selective electrode.

 

pH and Acidity in Wine by Automated Aliquoting

The pH value and the acidity in wine are determined with a combined pH glass electrode and by acid/base titration to pH value 8.2. The sample size is automatically adjusted by draining using a diaphragm pump.

 

Separation of Schizandrin, Schizandrin A, and Schizandrin B in a Tablet Sample

Hugan tablets, which contain Schisandra chinensis (Turcz.) Baill, are a traditional Chinese medicine for hepatoprotection. The major active components of Schisandra chinensis (Turcz.) Baill are lignanoids, and the three major lignanoids are schizandrin, schizandrin A, and schizandrin B.

 

Rapid Determination of Hesperidin in Orange Peel Using Accelerated Solvent Extraction and UHPLC

Hesperidin, the predominant flavonoid in orange peel and other citrus fruits, is an antioxidant that enhances the action of vitamin C to lower cholesterol levels, and is also known as an anti-inflammatory, antihistaminic, and antiviral agent.

 

Simultaneous Analysis of Water-Soluble Vitamins in Vitamin-Enriched Beverages and Multivitamin Dietary Supplements by UHPLC-MS/MS

Accurate quantitative measurements for vitamins are required to ensure product quality and regulatory compliance, as well as to monitor vitamin intake. Described here is a high-throughput UHPLC-MS/MS method for the simultaneous analysis of water-soluble vitamins in multivitamin supplements and vitamin-enriched beverages.

 

HPLC Analysis of Six Active Components of Caulis Lonicerae Using a Phenyl-1 Column

Caulis Lonicerae, the dried rattan of Lonicera japonica (honeysuckle family), is an important traditional Chinese medicine used for the treatment of ailments such as acute fever, headache, respiratory infection, and epidermic diseases.

 

Determination of Nitidine Chloride, Toddalolactone, and Chelerythrine Chloride by HPLC

The dried root Zanthoxylum nitidum (Roxb.) DC, an important traditional Chinese medicine, is regulated by the Pharmacopeia of the People’s Republic of China (PPRC) 2010 as an herbal remedy.

 

Rapid Separation of Anthocyanins in Cranberry and Bilberry Extracts Using a Core-Shell Particle

The methods described here provide a qualitative analysis of bilberry extract—a complex sample with 15 anthocyanins and five anthocyanidins—and a quantitative analysis of cranberry extract, both with a 20-minute time savings.

 

HPLC Separation of All-Trans-β-Carotene and Its Iodine-Induced Isomers Using a C30 Column

β-Carotene is generally regarded as the most commercially important and widely utilized carotenoid. It is used as a food coloring agent, antioxidant, and safe provitamin A source.

 

Mogroside V Determination by HPLC with Charged Aerosol and UV Detections

Luo han kuo fruit (Siraitia grosvenori Swingle) has long been used in traditional Asian medicine. Recently, cucurbitane-type and other triterpene glycosides isolated from the fruit are being investigated for numerous potential health benefits.

 

Determination of Sudan Dyes I–IV in Curry Paste

Sudan dyes are a class of synthetic dyes that are mainly used for industrial applications such as the coloring of plastic. These dyes are banned as a food-coloring agent because they are classified as carcinogens.

 

Determination of Phthalates in Drinking Water by UHPLC with UV Detection

Phthalates are a class of chemical compounds widely used as plasticizers for polyvinyl chloride resins, adhesives, and cellulose film coating. To date nearly 20 kinds of phthalates (structures shown in Figure 1) have been used for these purposes.

 

Simultaneous Determination of Tartaric Acid and Tolterodine in Tolterodine Tartrate

Tolterodine tartrate is a medication that is used to treat urinary urgency, thereby reducing the frequency of passing urine and urinary incontinence. Tolterodine, a quaternary ammonium compound, is the active pharmaceutical ingredient (API) and tartrate is the counterion in tolterodine tartrate.

 

Fully Automated Determination of The Permanganate Index in Accordance with DIN EN ISO 8467

Metrohm presents a method for completely automated determination of the permanganate index according to DIN EN ISO 8467 (DIN 38409-5). The determination of the permanganate index is a standard application performed in almost all water laboratories but keeping the quality of sample preparation consistent — including the time-critical heating of samples — is a challenge.

 

Determination of Formol Number, Acidity and True Brix in Orange Juice

A method for the determination of formol number (based on recommendations of DIN EN 1133 standard), acidity and true brix of grape and orange juice is presented.

 

Extraction Cortisol From Human Saliva Using ISOLUTE SLE+ Plates Prior to LC-MS/MS Analysis

This Application Note describes the supported liquid extraction clean-up of Cortisol from saliva prior to quantitative LC-MS/MS analysis. Cortisol is a steroid hormone that when measured from saliva can be used as an indication of stress.

 

Free Fatty Acids Content in Edible Oil

A method for the determination of the free fatty acids (FFA) content in edible oil by potentiometric titration with ethanolic potassium hydroxide in a non-aqueous mixture consisting of ethanol and diethylether (1:1 v/v) is presented.

 

Application of Bio-SPME for the Enrichment of Illicit Phenethylamine and Cathinone Compounds from Biological Samples

Recently the field of illicit drug testing has been met with a changing environment with the rapid development of unregulated designer and synthetic compounds. Of most concern has been the development of a class of phenethylamine and cathinone compounds being marketed as “Bath Salts, Jewelry Cleaner or Plant Food”.

 

Robust LC/MS Application for Bioanalysis of Pain Management Drugs


For efficient therapeutic drug monitoring, it is important for clinicians to have access to fast/ robust analytical methods for accurate assessment of drug efficacy. Industrial trends toward highly specific LC/MS applications over traditional ELISA type immunoassay has resulted in the need for highspeed chromatographic assays along with simplified sample preparation methods.

 

Determination of the Total Acid Number (TAN) using Thermometric Titration

The thermometric titration method presented here permits a simple and direct determination of the total acid number (TAN) in petroleum products.

 

Analysis of polycyclic aromatic hydrocarbons from vehicle exhaust using TD–GC/TOF MS

This Application Note describes how the BenchTOF-dx™ timeof-flight mass spectrometer and TargetView™ compound identiPcation software can be used to accurately identify tracelevel
polycyclic aromatic hydrocarbons (PAHs) in a complex vehicle exhaust particulate sample.

 

Analysis of Petroleum Fractions by ASTM D2887

ASTM method D2887 describes a simulated distillation protocol for the separation of petroleum fractions over the boiling points range of 55.5 to 538 °C. The Thermo ScientificTM TRACETM TR-SimDist GC column has been shown to achieve this separation in less than 20 minutes.

 

Analysis of 18 Polycyclic Aromatic Hydrocarbons in Soil Using the QuEChERS Method

The use of QuEChERS dispersive SPE as a simple, fast, and quantitative sample preparation method is demonstrated for the GC-MS analysis of 18 polycyclic aromatic hydrocarbons (PAHs) in soil. The suitability of the Thermo ScientificTM TraceGOLDTM TG-17SilMS GC column for the separation of 18 PAHs is also shown.

 

Analysis of Benzophenone and 4-Hydroxybenzophenone in Breakfast Cereal

The use of QuEChERS dispersive SPE as a simple, fast, and quantitative sample preparation method for the GC-MS analysis of benzophenone and 4-hydroxybenzophenone in breakfast cereal has been demonstrated. Additionally, the suitability of the Thermo Scientific™ TraceGOLD™ TG-17MS GC column for benzophenones analyses has been shown.

 

Analysis of Fatty Acid Methyl Esters (FAMEs) C8–C24 by FID Using a Metal Column

Fatty acid methyl ester (FAME) analysis is performed for a number of reasons, from measuring the fat content of foods to determining the constituents of biodiesel.

 

Analysis of Low Level Pyrethroid Pesticides in Water

A method for the determination of pyrethroids in water at ultra-low-level concentrations of 0.02 and 0.10 ng/mL was developed using solid-phase extraction (SPE) for pre-concentration and subsequent analysis by GC with PTV injection.

 

Extraction of Bath Salts (substituted cathinones) From Human Urine Using ISOLUTE SLE+ Columns prior to GC-MS Analysis

This application note describes the supported liquid extraction clean-up of a range of substituted cathinones from urine prior to quantitive GC-MS analysis.
‘Bath Salts’ is the street name for a family of designer drugs chemically similar to cathinones that give the user similar effects to amphetamines. the abuse of these drugs is on the increase and regulation against their use and supply has now been implemented in EU and North America.

 

Screening Workflows for Anticholinergic Drugs on the QTRAP® 5500 LC/MS/MS System

A combination of comprehensive drug screening, semiquantitation and confirmation is essential in the anti-doping industry. An ideal screening method should cover a large number of drugs, yield semi-quantitative results, and provide spectral information for confirmation– all in a single analysis.

 

Ultra-Sensitive Analysis of Aldosterone in Serum Using the AB SCIEX Triple Quad™ 6500 LC/MS/MS System

LC-MS/MS has become an important tool for the measurement of steroid hormones in clinical research studies. Historically, these analytes have been measured using GC-MS or immunoassays.

 

Simple LC-MS/MS Screening and Quantification Methods for the Analysis of 41 Common Pain Drugs in an Oral Fluid Matrix

Liquid Chromatography coupled to Tandem Mass Spectrometry (LC-MS/MS) is a widely used analytical tool for screening and confirmation of drugs of abuse in forensic samples. The detection of several compound classes, such as common pain panel and drugs of abuse is of much importance. While this analysis has generally been performed utilizing urine sample matrices, many research laboratories are investigating the analysis of these compounds in oral fluid matrices.

 

Rapid Separation of Analgesic Compounds Using a Solid Core HPLC Column

This application note demonstrates the use of a Thermo ScientificTM AccucoreTM Urea-HILIC column for the rapid analysis of the analgesic compounds aspirin, acetaminophen and salicylic acid.

 

Analysis of 3 Nonsteroidal Anti-inflammatory Drugs Using a Solid Core HPLC Column

Accucore HPLC columns use Core Enhanced TechnologyTM to facilitate fast and high efficiency
separations. The 2.6 μm diameter particles are not totally porous, but rather have a solid core and a porous outer layer. The optimized phase bonding creates a series of high coverage, robust phases. Accucore Polar Premium is an exceptionally rugged polar embedded reverse phase material that offers high efficiency, single run separation of polar and non-polar analytes. The specially designed bonded phase is stable from pH 1.5 to 10 and will not dewet in 100% aqueous mobile phase. The tightly controlled 2.6 μm diameter of Accucore particles results in much lower backpressures than typically seen with sub-2 μm materials.

 

Analysis of Estrogens Using a Solid Core HPLC Column

This application note demonstrates the use of the Thermo ScientificTM AccucoreTM Phenyl-X HPLC column for the analysis of aromatic steroids. When compared with a C18 column the Accucore™ Phenyl-X HPLC column provides high aromatic selectivity, good hydrophobic retention and unique, complementary selectivity.

 

Separation of a Mixture of Vitamin K Isomers Using a Solid Core HPLC Column at Sub-ambient Temperature

A high speed, high resolution separation of vitamin K1 and K2 was achieved on a Thermo ScientificTM AccucoreTM C30 column. The high shape selectivity of this phase enabled the separation of the cis/trans isomers of vitamin K1. The separation of the isomers is temperature dependent and is optimum at around 15 °C.

 

Total Sulphur Dioxide in Wines

The total amount of sulfur dioxide in wines is determined by redox titration with iodine as a titrant. Two techniques are illustrated: (1) the voltametric indication with a platinum double-pin polarized electrode, and (2) the standard potentiometric indication with a combined platinum ring electrode.

 

Determining The Water Content in Hand Cream

Application note L 492 provides a method for determining the water content in hand cream (hand balm).

 

Fully Automatic Determination of Sodium in Food Samples — Know The “True” Sodium Content

The analysis dicusses thermometric titration as a promising method for the straightforward sodium determination in foodstuffs. Thermometric sodium titration was tested for its applicability to various food matrices such as soups, gravy and several salty snacks. Enthalpy change can be monitored as a change in temperature of the solution using a sensitive digital thermometer.

 

Antibody Drug Conjugate (ADC) Analysis

Company: Wyatt Technology

There has been a significant resurgence in the development of antibody-drug conjugates (ADC) as target-directed therapeutic agents for cancer treatment. Among the factors critical to effective ADC design is the Drug Antibody Ratio (DAR).

 

Hyaluronic Acid (Polysaccharides)

Company: Wyatt Technology

Hyaluronic Acid (HA) is an ubiquitous, very high molar mass polysaccharide that has been of particular importance in ophthalmic surgery. HA acts as a molecular “shock-absorber” and stabilizer for cells and its visco-elastic properties are valuable for separating tissue and maintaining shape.

 

Supelco SLB®-IL60 Ionic Liquid GC Columns

The SLB-IL60 column is able to undergo the same analyte-phase interactions as polyethylene glycol (PEG) columns, but at different relative amounts. Based on its unique phase structure, the SLB-IL60 column is also able to undergo additional interactions that PEG columns cannot.

 

Increased Pigment Removal with Analysis of Pesticides in Oranges

Although pesticides have proven to be invaluable in crop production, the same toxicity, stability and mobility that enables them to effectively kill insects causes detrimental effects in humans.

 

EPA Method 525.2: Extraction of Semivolatile Organic Compounds from Water Using AutoTrace 280 Solid-Phase Extraction Cartridges

Traditionally, semivolatiles in drinking water have been extracted using liquid-liquid extraction techniques such as separatory funnel or continuous liquid-liquid extraction. Solid-phase extraction (SPE) is an alternative accepted extraction technique for USEPA Method 525.2 which uses significantly less solvent (up to 60 mL per sample).

 

An Improved HPLC Method for the Separation of Norethindrone and Mestranol with Progesterone as Internal Standard

This work demonstrates the use of a Thermo ScientificTM SyncronisTM 3 μm C8 column to produce effective separation of norethindrone, progesterone and mestranol giving equivalent results to those required from the USP method but in less time.

 

Analysis of Cephalosporins on a Polar Endcapped C18 3 μm Particle Column

The analysis of species containing polar groups using reversed phase HPLC can be challenging. The polar groups present on the analytes can result in secondary interactions with silanols on the silica surface.

 

Determination of Catechins and Phenolic Acids in Red Wine by Solid Phase Extraction and HPLC

This application note demonstrates a simple and rapid HPLC method for the analysis of nine catechins and phenolic acids in red wine. Extraction of these polar analytes was achieved on Thermo ScientificTM HyperSepTM Retain PEP material. The polyphenols in the extracts were quantified by a matrix-standard calibration, with extracts from a wine sample spiked with increasing amounts of analytes. Determination of the polyphenols was performed by HPLC, using a Thermo Scientific AccucoreTM PFP HPLC column under gradient mobile phase conditions.

 

Analysis of Non-Steroidal Anti-Inflammatory Drugs Using a Highly Pure, High Surface Area C18 HPLC Column

This application note demonstrates the use of the Thermo Scientific™ Syncronis™ C18 HPLC column for the analysis of non-steroidal anti-inflammatory drugs. Syncronis C18 columns provide a fast simple method with good hydrophobic retention, excellent peak shape and high
resolution.

 

Extraction of 1, 25 Dihydroxyvitamin D From Human Serum Using ISOLUTE SLE+ Prior to LC-MS/MS Analysis

This application note describes the supported liquid extraction of 1, 25 dihydroxyvitamin D2 and D3 from human serum prior to quantitative LC-MS/MS analysis.
This methodology has been designed to give an effective and efficient supported liquid extraction protocol for the clean-up and concentration of 1, 25 dihydroxyvitamin D2 and D3, important metabolites in the assessment of vitamin D deficiency.

 

Zinc, Nickel, Calcium and Magnesium in Borated Water of a Pressurized Water Reactor

In pressurized water reactors (PWRs), light water is used as primary coolant. Boron (as boric acid) readily absorbs neutrons and is added to the coolant to control reactivity. Lithium hydroxide assures a pH value greater than 7 to prevent corrosion. This application allows to measure sub-ppb levels of zinc, nickel, calcium, and magnesium besides high boric acid and lithium hydroxide
concentrations.

 

Chromate in drinking water by ion chromatography with PCR and UV/VIS detection according to EPA Method 218.7

Hexavalent chromium (chromate) is known to be cancerogenic if inhaled and suspected to be cancerogenic if ingested. EPA Method 218.7 allows to determine chromate in drinking water down to the sub-μg/L range (method detection limit, MDL = 15 ng/L). Post-column reaction with 1,5-diphenylcarbazide and subsequent visible detection at 530 nm is applied.

 

Monoclonal Antibodies and the Preparative Use of Flow Field-Flow Fractionation (AF4)

Company: Wyatt Technology

Proteins—especially monoclonal antibodies (MABs)— have become increasingly important in pharmaceutical work. However, there are some important differences between conventional, chemically-synthesized drugs and proteins. Because of the complex and weak structure of proteins, even a slight change in conditions, such as pH value, temperature or mechanical stress, may lead to aggregation and a loss of activity and/or stability.

 

Speciation of Iron(II) and Iron(III) Applying Post-column Reaction and Subsequent UC/VIS Detection

Speciation analysis is an important tool in analytical chemistry giving information about the quantitative distribution of different oxidation states of one and the same metal ion.

 

Reproducible Recoveries of Pesticides from Fruits and Vegetables

LC-MS/MS methods are become very popular for the analysis of pesticides in fruits and vegetables. This is due to their ability to resolve many analytes of varying functionality.

 

Analysis of Triglycerides in Butter and Lard

Triglycerides (also called triacylglycerol, triacylglyceride or TAG) are the main constituent of vegetable oil and animal fat, and make up most of the fats digested by humans.

 

Thermo Scientific Dionex Chromeleon 7 Chromatography Data System Software

System Suitability Testing (SST) is commonly used by laboratories to ensure that the complete analytical system (including instrument, reagents, columns and analysts) is suitable for the intended application.

 

Fast Analysis of Coffee Bean Extracts Using a Solid Core HPLC Column

It is believed that dietary phenols and polyphenols have the potential to protect the consumer’s health and as such there has been a great deal of research into plant products that contain these compounds. One rich source of these antioxidant compounds is coffee, where a range of chlorogenic acids is found.

 

Rapid Determination of Benzalkonium Chloride in a Cosmetic

Benzalkonium chloride (BKC), a typical quaternary ammonium salt, is often used as an antiseptic. Its structure is shown in Figure 1, and the C12 homolog is the major species in a benzalkonium chloride preparation.

 

LC-MS/MS Method for the Determination of Diclofenac in Human Plasma

A liquid chromatography-tandem mass spectrometry method for the determination of diclofenac in human plasma was developed. Using Thermo Scientific SOLA cartridges and plates, sample preparation was fast and efficient and gave excellent recovery levels for the compound.

 

Separation of a Mixture of PCBs Using an Accucore C18 HPLC Column

Polychlorinated biphenyls (PCBs) are man-made organic compounds composed of two phenyl (benzene ring) groups with multiple chlorine atoms attached. The heat-resistant and non-conductive properties of PCBs led to their extensive use as coolants and lubricants in electrical equipment until the late 1970s when their toxicity was recognized and their usage restricted. However, PCBs are very persistent environmental contaminants.

 

Analyzing Pesticide Residues in Lettuce by the EN 15662 Method using Phenomenex roQ™ QuEChERS Kits Followed by LC/MS/MS and GC/MS Analysis

The European Standard EN 15662 method for pesticide residues in foods is described for the analysis of 25 pesticides and 2 internal standards from lettuce using a Phenomenex roQ QuEChERS EN 15662 Extraction Kit and roQ dSPE Kit for sample preparation.

 

Rapid aroma profiling of cheese using a Micro-Chamber/Thermal Extractor with TD–GC/MS analysis

Hundreds of varieties of cheese are enjoyed by people around the world. The nature of cheese varies considerably, and the subtle differences in aroma, flavour and texture all add to its appeal. Various factors are involved in the nature of the final product, including the type of animal, its diet, processing of the milk, the cheese culture, and the ageing conditions.

 

Comprehensive analysis of aroma compounds from incense sticks using TD–GC/MS

Incense sticks (agarbatti) are used worldwide, but are especially popular in Asia. They are employed primarily in religious ceremonies, both in religious buildings and in the home, but also for aesthetic pleasure and in aromatherapy.

 

Analyzing PBDEs in House Dust Samples with the Thermo Scientific TSQ Quantum XLS Ultra GC-MS/MS in EI-SRM Mode

Polybrominated diphenyl ethers (PBDEs) were introduced in the 1960s as flame retardants and are currently used in a wide variety of household apparatuses, consumer electronics, furniture and more. Envir

 

Accelerated Solvent Extraction of Pesticide Residues in Food Products

Residue analysis in crops and food products is routinely performed in regulatory and industrial laboratories around the world. Many of the traditional procedures used to perform these extractions are time-consuming and solvent-intensive.

 

Rapid Determination of Fat in Meat Using Accelerated Solvent Extraction

Soxhlet extraction is an accepted technique for extracting fat from meat samples. Though it is simple and robust, there are drawbacks to Soxhlet extraction, such as long drying and extraction times, lack of automation, and the amount of solvent used per sample.

 

Simultaneous Extraction of PAHs and PCBs from Environmental Samples Using Accelerated Solvent Extraction

Accelerated solvent extraction is an established technique used for the extraction of solid and semisolid sample matrices using common solvents. Typical accelerated solvent extraction parameters include elevated temperatures and pressures, which enhance the kinetics of the
extraction process.

 

Extraction of Pain Management Drugs from Urine using EVOLUTE® CX With the RapidTrace+ Automated SPE Workstation Prior to LC-MS-MS

This application note describes the extraction of 21 different drugs in urine which are typically screened for pain management panels using EVOLUTE CX 100 mg/3 mL cartridges and automated using the RapidTrace workstation.

 

Extraction of Peptides From Human Plasma and Serum Using EVOLUTE® ABN 96-Well Plates Prior to LC-MS/MS

This application note describes the extraction of several peptides, ranging in size from a 7mer to a 54mer, from plasma and serum using EVOLUTE® ABN in a 96-well plate format.

 

Simultaneous Extraction of Ethyl Glucuronide and Ethyl Sulfate from Urine with EVOLUTE AX Prior to LC-MS-MS analysis

This application note describes the simultaneous extraction of the alcohol metabolites ethyl glucuronide (EtG) and ethyl sulfate (EtS) from human urine using EVOLUTE AX columns in a range of column sizes followed by LC-MS-MS analysis.

 

Characterization of Au Nanoparticles in a Complex Biological Matrix

Company: Wyatt Technology

There has been a remarkable surge in recent years in the use of nanoparticles in a variety of consumer products.

 

Transient Protein Self-Association Determined by SEC-MALS

Company: Wyatt Technology

Domain antibodies (dAbs) are the smallest functional binding units of antibodies, corresponding to the variable regions of either the heavy (VH) or light (VL) chains of human antibodies.

 

Polyvalent Pneumococcal Polysaccharide Vaccine (PNEUMOVAX®23)

Company: Wyatt Technology

An approach was developed to align release and end-expiry specifi cations for molecular size for the quality control of Merck’s polyvalent pneumococcal polysaccharide vaccine (PNEUMOVAX®23).

 

MALS + AFFF for Colloidal Drug Carrier Systems

Company: Wyatt Technology

Although gelatin provides important advantages, like its proteinacious structure and its biodegradability, there is one major drawback of gelatin that disturbs the manufacturing process. Related to the extraction of gelatin from collagen originating from different animal sources, its molecular weight distribution is very heterogeneous.

 

PEGylated Protein Modifications

Company: Wyatt Technology

Glycosylation and PEGylation are the most prevalent forms of protein modification. In the former, sugars are attached; in the latter, polyethylene glycol strands are connected as “whiskers” to increase the half-life of the protein and make it less likely to be hydrolyzed–or cleared–from the bloodstream.

 

Copper, Nickel, Zinc and Common Cations in The Water-Steam Cycle of a Boiling Water Reactor (BWR)

Water chemistry of the water-steam cycle is crucial for maintaining plant reliability and for ensuring optimal plant operational conditions. Impurities such as corrosion products in ionic, colloidal, or oxide forms are ubiquitous in feedwater, condensate, and reactor coolant.

 

Characterization of PLGA Using SEC-MALS-VIS

Company: Wyatt Technology

Poly(lactic-co-glycolic acid) (PLGA) is a copolymer based on glycolic acid and lactic acid. 

 

Automated Solid Phase Extraction (SPE)-LC-MS/MS Method for the Determination of Acrylamide in Brewed Coffee Samples

In this study, we show that a manual SPE method used for the determination of acrylamide in brewed coffee can be converted to an autosampler-compatible cartridge format and automated using a robotic autosampler controlled by user-friendly software. Calibration standards prepared in freshly brewed green coffee (unroasted) resulted in a linear calibration curve (r2=0.99) from 1 ng/mL to 500 ng/mL. Precision of the automated SPE-LC/MS/MS method was calculated as CV = 1.7 %.

 

Molecular Weight Determination of LMWH SEC/MALS vs. SEC/UV-RI

Company: Wyatt technology

Low-molecular-weight heparins (LMWHs) are obtained by fractionation or depolymerization
of natural heparins. They are defined as having a mass-average molecular weight of less than 8000 and for which at least 60% of the total weight has a molecular mass less than 8000.

 

Unattended Automated Standard Addition and Headspace Analysis for the Quantitative Determination of VOCs in Food Packaging

Headspace analysis by means of a dedicated autosampler is a standard technique for the determination of volatile organic compounds (VOCs) possibly present in food packaging materials. The packaging sample is typically cut into square pieces and placed in headspace vials for incubation at a determined temperature before the headspace sampling.

 

An Improved Fast RP-HPLC Method for Rosuvastatin and its Degradation Products Using a Thermo Scientific Accucore PFP HPLC Column

Rosuvastatin is classified as a statin, a type of agent that inhibits cholesterol production in the liver. Rosuvastatin calcium is a synthetic lipid-lowering agent approved as a treatment for hypercholesterolemia.

 

Concanavalin A Column for Analysis of Glycoproteins and Their Tryptic Glycopeptides

Glycosylation, one of the most common and complex post-translational modifications, is of great interest for its role in many biological processes such as molecular recognition, cell signaling, and immune defense.

 

Determination of Nitrite and Nitrate in Wastewater Using Capillary IC with UV Detection

Ion chromatography (IC) with suppressed conductivity detection is an effective technique to simultaneously determine common inorganic anions in environmental water and drinking water.

 

Automatic Precolumn Derivatization for the HPLC Determination of Aliphatic Amines in Air

Aliphatic amines such as methylamine, ethylamine, diethylamine, propylamine, and butylamine are considered important air pollutants due to their odorous and toxic properties.

 

Dramatically Improve Existing 5 μm and 3 μm Fully Porous Methods with Kinetex® 5 μm Core-shell Technology

With virtually no development effort or investment required chromatographers running traditional methods can instantly improve resolution, sensitivity, and productivity by simply replacing the 5 μm and 3 μm fully porous columns currently used with a Kinetex 5 μm core-shell column.

 

Fast Analysis of Water Pollutant Pesticides

A very fast gradient method for the simultaneous determination of 13 pesticides which are known to be important water pollutants is presented in this application note.

 

Automated USP and EP GPC/SEC Analysis of Low Molecular Weight Heparin (LMWH)

Natural heparin is a polysaccharide and consists of molecular chains of varying lengths. Low molecular weight heparin (LMWH) consists of short chains and is used as anticoagulant in diseases that feature thrombosis and for prophylaxis against it.

 

Online Analysis of Trace Anions in Power Plant Water Matrices

A setup that allows online sampling is crucial for immediate and contamination free analysis of power plant water samples.

 

A Single-Column Application For the GC Determination of Benzene in Reformulated Gasoline using a Supelco SLB-IL111 Ionic Liquid Column

The amount of benzene in gasoline is a concern because it is a known human carcinogen, and exposure to it has been linked to detrimental health effects. The challenge with the analysis lies in the complex composition of gasoline, which consists of hundreds of different compounds.

 

Determining The Water Content in Biodiesel

Biodiesel is produced from vegetable oil or animal fat by a reaction with methanol using a catalyst (KOH).

 

Analysis of Catechins Using a Thermo Scientific™ Accucore™ XL C8 4 μm HPLC Column

This application note compares the performance of a solid core  Accucore XL C8 4 μm HPLC column with that of a fully porous 5 μm  traditional HPLC column for the analysis of catechins under gradient  mobile phase conditions.
 

Analysis of Triazines Using a Thermo Scientific™ Accucore™ XL C8 4 µm HPLC Column

This application note compares the performance of the solid core Accucore XL C8 4 µm HPLC column with that of a fully porous 5 µm traditional HPLC column for the analysis of triazines under gradient mobile phase conditions.  

 

Analysis of Ibuprofen and Valerophenone Using a Thermo Scientific™ Accucore™ XL C18 4 µm HPLC Column

This application note compares the performance of the solid core Accucore XL C18 4 μm HPLC column with that of a fully porous 5 μm traditional HPLC column for the analysis of ibuprofen and valerophenone using a isocratic method based on the USP.

 

Analysis of Fat Soluble Vitamins Using a Thermo Scientific™ Accucore™ XL C18 4 µm HPLC Column

Based on Core Enhanced Technology™ using 4 µm solid core particles, Accucore XL HPLC columns allow users of conventional HPLC methods to enjoy performance far beyond that of columns packed with 5 µm or even 3 µm fully porous particles.

 

Analysis of Endocrine Disruptors Using a Thermo Scientific™ Accucore™ XL C8 4 µm HPLC Column

This application note compares the performance of the solid core  Thermo Scientific Accucore XL C8 4 µm HPLC column with that of a  fully porous 5 µm traditional HPLC column for the analysis of endocrine  disruptors under gradient mobile phase conditions.
 

Analysis of Intact Proteins on a Thermo Scientific™ Accucore™ 150-C4 150 Å Pore Diameter HPLC Column

This application note demonstrates the analysis of intact proteins using an Accucore 150-C4 (150 Å pore diameter) HPLC column. The analysis of six proteins ranging in mass from 6 to 45 kDa is carried  out in 15 minutes with pressures compatible with conventional HPLC  instrumentation. Excellent loading capacity was observed for this column.

 

LC-MS/MS Method for the Determination of Testosterone using a Thermo Scientific™ Accucore™ C8 HPLC Column

A liquid chromatography-tandem mass spectrometry method for the analysis of testosterone was carried out on an Accucore C8 HPLC Column (2.6 µm 50 x 2.1 mm) resulting in a fast separation with a cycle time of 1.5 minutes while maintaining excellent peak shape.

 

Reversed-Phase Analysis of a Monoclonal Antibody on an Accucore C4-150 HPLC Column

Accucore HPLC columns use Core Enhanced Technology to facilitate fast and highly efficient separations. The 2.6 μm diameter particles are not totally porous but have a solid core and a porous outer layer. 

 

Bruker Newsletter #1: Ion Trap MS

Modern ion trap systems offer rock solid advantages to the user in a rapidly changing world of mass spectrometry. Incredibly easy to use and of outstanding robustness they deliver the fastest MSn results at all-time sensitivity.

 

Method Transfer between HPLC and UHPLC Instruments: Equipment-related challenges and Solutions

Today, ultra-high-performance liquid chromatography (UHPLC) has taken a firm foothold in the analytical laboratory. However, it is rare that 100% of instrumentation within a company is all from the same vendor and of the same model.

 

Interlaboratory Tests Demonstrate the Robustness and Transferability of the Toxtyper Workflow

Here we describe a robust and automated research based screening solution for the detection and identification of drugs and drugs of abuse in biological specimens. The workflow was tested with regard to method- and result-transferability from lab to lab.

 

Toxtyper – a Comprehensive LC-MS Screening Solution for Clinical and Forensic Toxicology

Here we describe a robust and automates research based screening solution based on the latest LC-MSn ion trap technology that promises to provide a combination of the highest performance LC-MS/MS and easy-to-use identification with the greatest transferability of results from lab to lab.

 

Separation of clindamycin phosphate and process impurities

In this application note an isocratic UHPLC separation of clindamycin phosphate from its precursor product lincomycin and impurities like clindamycin is presented.

 

Authenticity Assessment of Fruit Juices using LC-MS/MS and Metabolomic Data Processing

In this study, the feasibility of LC-MS/MS techniques employing Q TRAP and TripleTOF systems for metabolomic-based authentication of fruit juices (including apple, blueberry, cranberry, grapefruit, orange, pomegranate, and their mixtures) was explored.

 

Enhancing the development of low-emitting products and materials

This Application Note describes how sampling technologies for thermal desorption that are typically used by test laboratories for screening products for chemical emissions can also provide manufacturers with tools that greatly aid the development of low-emitting products and materials, and thus compete in the expanding market for ‘green’ products.

 

Improved Resolution of Triazine Herbicides with Kinetex Core-Shell HPLC/UHPLC Columns and Zebron GC Columns

Environmental laboratories are continuously pushed to deliver lower detection levels and faster sample throughput. A common analysis performed by these labs is triazine herbicides. This analysis can be performed by LC/MS/MS or GC/MS, for which Kinetex core-shell UHPLC/HPLC columns and Zebron GC columns provide resolution and sensitivity improvements as well as time savings.

 

Relevant Parameters in Developing Protein Aggregation Methods Using Yarra GFC Columns

A new high efficiency GFC column, Yarra, was recently introduced and is significantly more efficient than other GFC columns on the market. In addition to higher efficiency, Yarra columns demonstrate significantly higher inertness to ionic interactions versus other GFC columns; however, such chemical characteristics sometimes require changes to operating parameters. Performing method development for protein aggregation analysis using next-generation Yarra GFC columns will be discussed.

 

Determination of pesticides by UHPLC-MS

In this application note we present a method combining the rapidness of a UHPLC separation with the advantages of mass spectrometry detection.

 

Molar Mass and Chemical Composition 2D Analysis for Thermoplastic Elastomers

Gradient HPLC can be hyphenated with GPC/SEC in a fully automated setup to measure molar mass and chemical composition distribution of copolymers simultaneously with highest peak capacity.

 

Targeted and Non-Targeted Screening for Drugs with High Confidence using the AB SCIEX TripleTOF 4600 System and Intuitive Data Processing tools

The high resolution and accurate mass AB SCIEX TripleTOF 4600 LC/MS/MS system was used to screen for drugs from forensic equine urine, and to quantify drug compounds with excellent accuracy and high reproducibility.

 

The Use of Micro Flow UHPLC in Pesticide Screening of Food Samples by LC-MS/MS

Here we present new data using Eksigent ekspert microLC 200 System in combination with a LC-MS/MS method developed on an AB SCIEX QTRAP 4500 system and utilizing the Scheduled MRM algorithm to maximize the number of data points across each peak.

 

Derivatization Reagents: For Selective Response and Detection in Complex Matrices

Derivatization is a commonly used technique to augment chromatography analysis. It requires efficient and effective reagents that can modify the behavior of complex compounds and allow their detection in chromatographic analysis.

 

Determination of Bisphenol A in Drinking Water

A comprehensive sample preparation and analytical procedure was developed for determining BPA in drinking water. This fast procedure employed materials and techniques selected in part for speed, but also those that would not contribute unwanted artifacts.

 

Sampling of Carbonyls Using a Dual-Layer LpDNPH Glass Sampling Tube and HPLC Analysis With an Ascentis Express C18 Column

The dual-layer LpDNPH sorbent tube is an air sampling device designed for sampling carbonyls (e.g. formaldehyde) in ambient, indoor, and industrial atmospheres. Carbonyls are trapped on our high-purity silica gel adsorbent coated with 2,4-dinitrophenylhydrazine (2,4-DNPH) where they are converted to stable hydrazone derivatives. 

 

Leveraging Column Selectivity in Method Development for Illicit Amphetamines

The ability of LC-MS and UHPLC-MS experiments to provide valuable information for compound identification is enhanced by the often-overlooked power of bonded phase selectivity. In this first part of a series on LC-MS optimization that we will publish in The Reporter, we demonstrate the use of bonded phase selectivity for the analysis of illicit street amphetamines, also known as bath salts.

 

Comprehensive Determination of Trans Fats in Cookies using SP-2560 and SLB-IL111 GC Columns after Silver-Ion SPE Fractionation

In this application, we have demonstrated the extraction of lipids as fatty acids, and subsequent detection of trans fats from a cookie sample made using partially hydrogenated vegetable oils.

 

Improved Recovery of the Fungicide Carbendazim from Various Orange Juice Matrices by Employing QuEChERS Cleanup

Fungicide carbendazim can some times be used to combat mold on citrus fruits including oranges. Recently, low residue levels of the fungicide were reported to be present in the bulk orange juice import shipments to the USA.

 

Analysis of Triazines Using a Thermo Scientific Accucore XL C8 4 μm HPLC Column

This application note compares the performance of the solid core Thermo Scientific Accucore XL C8 4 μm HPLC column with that of a fully porous 5 μm traditional HPLC column for the analysis of triazines under gradient mobile phase conditions.

 

Analysis of Endocrine Disruptors Using a Thermo Scientific Accucore XL C8 4 μm HPLC Column

This application note compares the performance of the solid core Thermo Scientific Accucore XL C8 4 μm HPLC column with that of a fully porous 5 μm traditional HPLC column for the analysis of endocrine disruptors under gradient mobile phase conditions.

 

A Novel Approach to the Certification of Pharmaceutical Reference Standards: Amino Acids by HPLC-Evaporative Light Scattering Detector

Traditional methods used to assess purity of amino acids are problematic in that they tend to be non-specific and/or semi-quantitative at best. Classically, the assay method for amino acids has been a titration procedure. Since typical impurities in an amino acid are themselves similar amino acids, they may give a similar titration response, thus overestimating the assay value of the main component. 

 

Determination of Nitidine Chloride, Toddalolactone, and Chelerythrine Chloride by HPLC

Zanthoxylum nitidum (Roxb.) DC is an important traditional Chinese medicine. The Pharmacopeia of the People’s Republic of China (PPRC) 2010 regulates this dried root as an herbal medicine. Nitidine is the specifi c active component in the dried root version of Zanthoxylum nitidum (Roxb.) DC, and nitidine chloride is reported to be beneficial for both killing and constraining the growth of cancerous cells.

 

Separation of Metformin and Voglibose Using a Thermo Scientific Accucore HILIC HPLC Column

This application note demonstrates the use of the Accucore HILIC HPLC column for the separation of two highly polar anti-diabetic drugs, metformin and voglibose.

 

LC-MS/MS Method for the Determination of Testosterone using an Accucore C8 HPLC Column

A liquid chromatography-tandem mass spectrometry method for the analysis of testosterone was carried out on a Thermo Scientific Accucore C8 HPLC Column, 2.6 μm 50 x 2.1 mm resulting in a fast separation with a cycle time of 1.5 minutes while maintaining excellent peak shape.

 

Separation of Phospholipids Derived from Biological Extracts Using a Solid Core Reversed Phase HPLC Column

In this application a Thermo Scientific Accucore RP-MS LC column was used to separate a range of lipids derived from biological sources. Excellent chromatographic performance was achieved at backpressures comparable with conventional HPLC instrumentation. The Accucore RP-MS HPLC column is an ideal phase for lipid analysis due to the balance of speed and efficiency. It utilizes core enhanced technology with optimized bonding for reversed phase HPLC and LC-MS analysis.

 

Analysis of Ibuprofen and Valerophenone Using a Thermo Scientific Accucore XL C18 4 μm HPLC Column

This application note compares the performance of the solid core Thermo Scientific Accucore XL C18 4 μm HPLC column with that of a fully porous 5 μm traditional HPLC column for the analysis of ibuprofen and valerophenone using a isocratic method based on the USP.

 

InertCap Pure-WAX

This application note shows how there is no need for ion chromatography for the separation of acetic acid in Class 3 compounds if using the InertCap Pure-WAX. (GL Sciences)

 

Determination of Melamine and its Analogues from Powdered Infant Milk Using Polymeric Solid Phase Extraction

Since the infant milk scandal in 2007, several methods have been released for the analysis of melamine from dairy products. However, a comprehensive method for the analysis of the related compounds (ammeline, ammelide, and cyanuric acid) is difficult to find.

 

The Detection of Allergens in Bread and Pasta by Liquid Chromatography Tandem Mass Spectrometry

A rapid, robust, sensitive and specific LC-MS/MS assay has been developed for the simultaneous detection of four major food allergens peanut, milk, wheat and egg. Peptides of allergens were detected at low parts-per-million (ppm) levels after simple homogenization, digestion with trypsin and SPE cleanup.

 

Analysis of Residual Pesticides in Processed Foods Using GC-MS/MS

This application datasheet presents a study of an analysis of residual pesticides in retort-packed curry using QuEChERS and GC-MS/MS. QuEChERS method is commonly used for vegetables due to its speed and simplicity. While GC-MS/MS is able to selectively separate residual pesticides from a large quantity of co-extracted substances.

 

Analysis of the Mycotoxin Patulin in Apple Juice

This application note will demonstrate a rapid method for the identification and quantification of patulin in apple juice using high performance liquid chromatography with UV detection.