Services Provided

Method Development and Validation

NDA Analytics can develop methods for both drug substance (API) and drug product, including active ingredient, related impurity and excipient assays and methodology for performance characteristic tests (e.g. dissolution). Undertaking method development requires close co-operation with our customers, who are requested to provide background data on the compound and product (although, if necessary, NDA Analytics can determine physicochemical properties, such as boiling/melting point, partition coefficient, solubility, spectral data and pKa).

For stability studies, stability-indicating methods are essential. It may be that a single method can be demonstrated to be stability-indicating, but sometimes a combination of methods (e.g. HPLC on different column chemistries or HPLC combined with an electrophoretic technique) is necessary. If the customer already has information on the degradation pathways and/or reference materials for degradation products, these can be used to demonstrate that a method is stability-indicating, otherwise NDA Analytics may need to elucidate these by stress testing and subsequent identification of degradates (another service that NDA Analytics can provide).

Methods development includes establishment of system suitability criteria and stability of laboratory solutions and samples and takes into account any relevant pharmacopoeia requirements.

With method development studies, it is usual to agree objectives, milestones and blocks of work in advance with the sponsor. At each milestone and/or at the end of each block of work, NDA Analytics reports progress to the sponsor and agrees further work if necessary.

Method Validation

ICH Q2A defines the terminology for validation, i.e. accuracy, precision, intermediate precision, LOD, LOQ, etc. ICH Q2B details how these parameters should be determined and calculated, e.g. number of replicate assays and number of levels for both drug substance and drug product.

The guidelines cover validation requirements for NDA and MAA submissions. However, validation can be tailored to the stage that a product is at in the development cycle. Limited validation can be submitted for clinical trials, i.e. IND and CTA. NDA Analytics can provide both full and tailored validation studies, depending on data requirements.