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Oligonucleotide Therapeutics Analysis: Methods for Drug Development and GMP Compliance

Mastering oligonucleotide therapeutics analysis requires advanced techniques for the analysis of oligonucleotides and related substances to meet regulatory standards and achieve product excellence.
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AI-driven pharmaceutical analysis concept showing digital intelligence applied to drug discovery and quality control, highlighting advanced methods for oligonucleotide therapeutics analysis in biopharma.

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As oligonucleotide drugs enter mainstream clinical use, analytical laboratories face new pressures to deliver reliable and compliant results with efficiency. These oligonucleotide therapies, targeting genetic disorders, viral infections, and cancers, introduce unique analytical challenges due to their structural complexity and evolving regulatory demands.

For quality control (QC) teams, the stakes are high. Oligonucleotide therapeutics analysis requires precise monitoring of sequence integrity, impurity profiles, and product consistency to meet Good Manufacturing Practice (GMP) standards. Any gaps in analytical performance could compromise product quality and delay regulatory approval.

This article presents a workflow-driven approach to meet these challenges, covering every phase of oligonucleotide analysis—from purification to final release testing—to help ensure success in regulatory submissions and patient outcomes.

Facing Challenges in Oligonucleotide Therapeutics Analysis 

Understanding the analytical complexities of oligonucleotide therapeutics analysis is essential for developing robust, regulatory-compliant workflows, and successfully navigating these hurdles requires a deep understanding of each technique's strengths and limitations.

Oligonucleotide Molecular Complexity, Structural Heterogeneity, and Impurity Profiling

Oligonucleotides often incorporate chemical modifications and secondary structures that complicate analysis. Their inherent instability and susceptibility to degradation result in impurities such as truncated sequences and oxidative byproducts, which must be reliably detected and quantified.

Overcoming Analytical Challenges in Oligonucleotide QC Across Technologies

Each oligonucleotide analysis technique presents unique challenges. For example, methods such as liquid chromatography (LC) and mass spectrometry (MS) face issues related to polarity, metal interactions, and complex ionization behaviors, which can affect detection and quantification. Meanwhile, separation methods such as capillary electrophoresis (CE) may struggle with matrix effects, and approaches including ultraviolet-visible (UV-Vis) spectroscopy or quantitative PCR (qPCR) offer limited insight into structural features or impurity profiles. Even advanced techniques such as next-generation sequencing (NGS) require extensive preparation and sophisticated data analysis.

To overcome these challenges, laboratories should adopt a holistic, multi-technique analytical strategy. By combining complementary methods, it becomes possible to offset the limitations of individual approaches and ensure accurate, reproducible results.

Oligonucleotide Analytical Workflows: From Purification to GMP-Compliant Product Release

Selecting the right technique for each stage is critical to building a robust workflow that delivers accurate, actionable data and meets regulatory expectations. Below, we outline each major step in the process and the best-fit analytical techniques that support them.

  • Identity and purity: ion-pair reversed-phase HPLC (IP-RP HPLC) is foundational for separating oligonucleotide variants and quantifying impurities. It also supports preparative scale-up for GMP production.
  • Structural confirmation and impurities: MS complements HPLC by confirming molecular identity, detecting modifications, and profiling impurities that may not be chromatographically resolved.
  • Impurity profiling: CE offers high-resolution separation of charge and size variants, serving as an orthogonal method to LC and MS.
  • Final quantification and integrity: UV-Vis spectroscopy with qPCR enables rapid concentration determination and verifies synthesis yield and sequence integrity, respectively, ensuring readiness for batch release.

Each analytical method plays a distinct role within a comprehensive workflow, contributing to the accuracy and compliance of oligonucleotide QC.

Oligonucleotide Analytical Techniques Compared: Impurity Profiling, QC, and Regulatory Fit

Selecting the right analytical technique for each stage of oligonucleotide analysis is critical, but how do these methods compare in terms of practical performance? The table below offers a side-by-side view of key attributes to help laboratories make informed decisions when building or refining their QC workflows.

Table 1: Oligonucleotide Therapeutics Analysis Methods Compared: Speed, Accuracy, Compliance, and Throughput

Technique

Speed

Accuracy

Regulatory Fit

Cost

Throughput

Ion-Pair Reversed-Phase HPLC

Moderate–High

Excellent for purity/impurity profiling

Standard QC method

Moderate

High

Mass Spectrometry (MS)

High

Excellent for identity and modification detection

Critical for structure and impurities 

High

Moderate

Capillary Electrophoresis (CE)

Very High

High for charge/size variants

Accepted complementary QC method

Low-Moderate

Very High

Next-Generation Sequencing (NGS)

Moderate

Unparalleled sequence fidelity

Emerging method for early-phase/research

Very High

Moderate

UV-Vis Spectroscopy

Very High

Reliable for concentration measurement

Routine QC standard

Low

Very High

Quantitative PCR (qPCR)

High

High specificity for sequence verification

Increasingly used for integrity testing

Moderate

High

A strategic mix of complementary techniques allows laboratories to offset method-specific limitations, boost accuracy, and meet both regulatory and operational demands. This integrated approach is essential for building a GMP-compliant framework that ensures consistent quality from development through release.

Incorporating Digital Tools to Streamline Oligonucleotide Therapeutics Analysis and GMP Compliance

As QC demands increase, laboratories are turning to digital tools such as analytical data processing systems, laboratory information management systems (LIMS), and Quality management software (QMS) to do the following:

  1. Automate QC workflows: Specialized data analysis platforms automate impurity profiling and peak integration. By reducing manual steps, these tools minimize variability and improve efficiency.

  2. Ensuring data integrity and compliance: In regulated environments, digital tools secure data handling with audit trails and electronic signatures, ensuring compliance with documentation regulations.

  3. Optimizing oligonucleotide-specific analysis tasks: Tailored specifically for oligonucleotide analysis, OAA eliminates the need for extensive customization, accelerating analysis while preserving data integrity.

Purpose-built digital tools streamline oligonucleotide QC, reducing turnaround times and reinforcing regulatory readiness.

Emerging Trends in Oligonucleotide Therapeutics Analysis: NGS, Bioinformatics, and AI in QC

As the field of oligonucleotide therapeutics evolves, analytical methods must also advance to meet new regulatory expectations and research demands. Several emerging technologies and approaches are shaping the future of oligonucleotide analysis, offering opportunities to enhance data accuracy, improve workflow efficiency, and support the next generation of drug development:

  • NGS and bioinformatics: NGS delivers unmatched sequence fidelity and minor variant detection. As regulatory agencies emphasize data integrity, NGS is poised to play a larger role in late-phase development and release testing. Machine learning and bioinformatics are also emerging to automate impurity classification and improve decision-making.
  • High-throughput and bio-inert chromatography solutions: New chromatography formats support LC-MS workflows and reduce oligonucleotide-metal interactions.

Future-ready labs should prepare for increased adoption of NGS and AI-enhanced analytics to meet regulatory and throughput demands.

Building a GMP-Ready Analytical Framework for Oligonucleotide Therapeutics Analysis

Oligonucleotide analysis requires a multi-faceted approach that integrates advanced chromatography, electrophoresis, mass spectrometry, and digital tools.

By aligning each technique with its optimal workflow stage and adopting purpose-built software, laboratories can:

  • Achieve accurate impurity profiling and sequence verification
  • Ensure regulatory compliance and data integrity
  • Increase efficiency and reproducibility in batch release testing

Forward-looking labs that embrace these best practices will be best positioned to meet evolving regulatory demands and support the future of oligonucleotide-based medicine.

Meet the Author(s):

  • Shiama Thiageswaran is an Assistant Editor at Separation Science. She holds a Master’s degree in Biochemistry and Molecular Biology, and has a research background in assisted reproductive biotechnology.

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