Analytical method development, verification and validation to cGMP

We have wide experience in method development for the the pharmaceutical, medical device and healthcare industry sectors, including working with clients carrying out method validation work to meet regulatory requirements, and for internal cGMP needs.

Method development

We agree an approach with the client, usually in discrete costed sections to control the overall programme cost. The work can include developing a test method from scratch, or changing/improving existing methods. Our experience includes, small and large molecules, also polymers, plastics, bone substitute and similar medical device products, as well as nicotine-based products.

We develop methods in the following broad areas:
  • Liquid and gas chromatography (for example, for stability indicating methods, residual solvents)
  • Materials characterisation/solid state
  • Wet chemistry

All projects are documented with a final report, including a final write up of the method, and typically with inclusion into our Controlled Documentation systems.

Method validation

Method validation is a process that usually starts with an in-house single validation exercise which can then progress to validation at multiple sites and then to standardised publication.

We are happy to produce our own Validation Protocols, or work to formats provided by our client.  After execution of the protocol results are provided as a final method validation report in line with the protocol, with the method details included or referenced. Typical test method validation parameters are based on ICH guidelines (for example robustness, linearity, limit of detection, limit of quantitation, accuracy, precision, and specificity) or as agreed with the client.

Our validation methods include:
  • HPLC (assay and impurities methods, cleaning verification methods)
  • Liquid injection chromatography (solvent identification and release test methods)
  • Headspace gas chromatography (residual solvent analysis)
  • Physical methods such as Malvern sympatec particle sizing, specific surface area by BET and XRPD
  • Trace and major elemental determination by ICP-OES and X-ray fluorescence and total organic carbon analysis
  • API raw material and chemical intermediate methods (Karl Fischer, titration, loss on drying, residue on evaporation)

Method verification

Method verification is used to demonstrate that a standardised published method can be run effectively in each laboratory.

The requirements for method verification are less stringent than for validation but the principle approach is the same. A formal Verification Protocol with defined acceptance criteria is produced and agreed with the client (the client always agrees and signs the protocol). The verification is then executed and reported in a Verification Report, with the method details included or referenced.

The extent of the verification will depend on the procedural and sample complexity but as a minimum the verification will require demonstration that the performance parameters (for example system suitability tests) specified in the method have been met with the matrices to which the method is being applied (typically analyte recovery assessment).  For HPLC assay methods it is sometimes necessary to carry out a limited linearity assessment due to flow cell differences.

Our verification methods include:
  • HPLC (assay and impurities methods, cleaning verification methods)
  • Liquid injection chromatography (solvent identification and release test methods)
  • Headspace gas chromatography (residual solvent analysis)
  • Physical methods such as Malvern sympatec particle sizing, specific surface area by BET and XRPD
  • Trace and major elemental determination by ICP-OES and X-ray fluorescence and total organic carbon analysis
  • API raw material and chemical intermediate methods (Karl Fischer, titration, loss on drying, residue on evaporation)

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