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.

Comments

Post a Comment

Popular posts from this blog

Understanding Quantitative, Qualitative, and Limit Tests in Pharmaceutical Quality Control

In pharmaceuticals, quantitative, qualitative, and limit tests refer to different approaches for analyzing drugs and their components: 1 . Quantitative Test: This determines the exact amount or concentration of a specific substance in a pharmaceutical product. It provides precise measurements, such as the amount of active pharmaceutical ingredient (API) or impurities present. For example, assays like High-Performance Liquid Chromatography (HPLC) are used to quantify substances. 2. Qualitative Test: This identifies the presence or absence of a particular substance but does not measure its amount. These tests confirm the identity of the compound, ensuring that the correct API is present. Techniques such as Infrared (IR) spectroscopy or Thin Layer Chromatography (TLC) can be used for qualitative analysis. 3. Limit Test: This is a type of semi-quantitative test used to check whether the concentration of a substance (like impurities) in a sample is within prescribed limits. It doesn’t prov...
Read more

USFDA Inspection Types

The FDA and States assisting the FDA under contract or cooperative agreements, in general, perform three types of inspections: surveillance, compliance follow up, and for-cause. Surveillance inspections are conducted to assess a facility’s or farm’s compliance with a regulation or to focus on an emerging trend in food safety. Surveillance inspections fall into two categories, routine and targeted. Routine inspections of facilities and farms are conducted to assess regulatory compliance. The FDA Food Safety Modernization Act mandates an inspection frequency of at least once every three years for domestic high-risk facilities and at least once every five years for non-high-risk facilities. In addition, the Food and Drug Omnibus Reform Act of 2022 mandated annual inspections of infant formula manufacturers in accordance with a risk-based approach. If necessary, inspections can be conducted more frequently. The FDA seeks to achieve comparable coverage of imported foods using an array of re...
Read more

Handling of Market Complaints and Their Importance in the Pharmaceutical Industry

In the pharmaceutical industry, market complaints serve as a critical feedback mechanism that helps maintain the safety, quality, and efficacy of products. Efficient handling of these complaints not only protects patient health but also strengthens the company's reputation and regulatory compliance. This blog post is to explore the importance of market complaints and best practices for managing them effectively. The Importance of Market Complaints Ensuring Patient Safety The primary objective of pharmaceutical companies is to provide safe and effective products to patients. Market complaints, especially those related to adverse drug reactions or product defects, can indicate potential risks. Immediate investigation and corrective action help prevent further harm to patients. Maintaining Product Quality Market complaints can reveal issues with the product’s quality, such as impurities, packaging defects, or labeling errors. Addressing these complaints promptly ensures that quality i...
Read more