Steps involved in analytical method validation

 Analytical method validation is one of the most important activity in product life cycle.

I have tried to summarize steps involved in method validation.

Step-1: Preparation of method of analysis: Based upon final method development experiment and upon confirmation of few critical validation parameters (such as precision, accuracy, forced degradation etc...), you need to prepare final method of analysis.

Step-2: preparation of Specification: Upon finalization of process and formula for product, now it is time to prepare specification. The specification must be prepared in consultation with pharmacopoeia of target geography, critical process and product attributes and any additional regional requirement. 

Step-3: Preparation of concentration matrix: Before heading to protocol preparation, it is highly important to map the concentration of sample and standard for various method validation parameters. Concentration matrix gives huge guidance on preparation of various solutions, their concentrations and much more. It also become one of the most important guiding document during protocol preparation.

Step-4: Preparation of protocol: Protocol is one of the most important document related to validation. The protocol must be prepared in consultation with ICH guideline for method validation. The method of analysis, specification and concentration matrix shall be referred while protocol preparation. 

Step-5: Pre-requisites: The availability of placebo, sample, standards, impurities, chemicals/reagents, columns (in case of HPLC/GC method) must be thoroughly confirmed. 

Step-6: Execution: The execution is one of the key factor in determining completion of validation activity. The deviation/incidents occurred during execution must be addressed immediately and appropriately.

Step-7: Calculation & Conclusion: Each and every parameter must be assessed once the experiment is over. The delay in calculation may lead to repeat experiment and non-conformity

Step-8: Preparation of method validation report: Upon successful execution, the summary report can be prepared. The summary report shall consist of actual results and conclusion.