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Method development /validation

Method development

HHAC can draw on over 20 years’ experience in method development, a period in which various methods for testing quality-indicative parameters of active substances and finished medicinal products were performed for more than 350 different active substances.

Irrespective of the task at hand, i.e. release testing, stability testing (e.g. identity, assay, purity, residue analysis, residual solvent analysis or active substance release ) or analytical procedures (high performance liquid chromatography [HPLC], high performance liquid chromatography-mass spectrometry [HPLC-MS], gas chromatography [GC], ultraviolet-visible spectroscopy [UV-VIS], Karl-Fischer titration, thin-layer chromatography [TLC], etc.), we develop tailor-made methods for our clients.

This applies to solid, semi-solid and liquid dosage forms, synthetic or herbal medicinal products and raw materials.

We aim to provide robust methods for routine operation.

After a method has been developed or optimised, it undergoes comprehensive, state-of-the-art validation in compliance with the validation protocol and, in particular, with the ICH guidelines. Client-specific standard operating procedures (SOPs) are, of course, also taken into consideration.

Method validation

When validating purity, assay and release methods, we determine the necessary scope of validation, in close collaboration with our client. The method is specifically tested for the effect of critical parameters with respect to robustness (risk assessment). When performing controlled degradation studies for purity methods, particular consideration is given to influencing variables such as light and heat, and oxidative, acidic and alkaline stress.

After the risk assessment, acceptance criteria are determined and stipulated in the validation protocol.

Of course, we also perform validation of pre-existing methods in accordance with the client’s own validation protocols.

Validation parameters:

ParametersIdentityImpuritiesAssay
QuantitativeLimit test
Accuracyxx
Precision
Precision repeatabilityxx
Reproducibility1xx
Specificity/selectivity2xxxx
Limit of detection "LOD"3x
Limit of quantitation "LOQ"x
Linearityxx
Rangexx


1 If a laboratory comparison is performed, the reproducibility or "intermediate precision" is not carried out
2 Lack of specificity can be compensated for by a second procedure
3 Necessary in certain cases

Validation report

The work concludes with the compilation of a validation report. The client receives a comprehensive validation report, in German or English, and all the necessary validation data are made available.

Depending on the project’s complexity, our client receives a draft version of the validation report, in order to ensure agreement.

Validated methods are verified after installation in compliance with USP <1226>. This ensures correct use of the method and it can be promptly incorporated into routine operations.

After successful method development and validation, a rapid and smooth method transfer is ensured, so that the validated method can be promptly used.