A Step-by-Step Guide for Method Validation
What is Validation? •
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
•
Validation is a process-risk will determine the effort
High Risk
Moderate risk
Low risk
• Total validation
• Testing, documentation
• Testing the change
Validation of Analytical Methods-Key Steps Preparation
Experimentation
Transferring method
Documentation
Step 1- Preparation • Develop validation project plan • Define purpose/scope of method (performance criteria) • Define and verify performance of equipment • Qualify/validate materials • Qualify/train operator
Step 2- Experimentation • Perform validation experiments- may have to change either equipment or limits • Develop SOPs for executing the method in routine • Define type and frequency of system suitability tests and/or analytical quality control (AQC) checks • Define change control procedure • Document validation experiments and results
Step 3- Transferring Methods to Routine Laboratories • Designate project owner • Develop procedure on how to use method • Develop system suitability tests (test procedure, frequency, acceptance criteria) • Define transfer tests and acceptance criteria in the routine • Train routine lab analyst in development lab • Repeat 2 critical method validation tests in routine lab • Analyze at least three samples in development and routine lab • Analyst in routine lab should give frequent feedback
Step 4- Documentation for the FDA Validation report and supporting documentation: • Objective, scope • Methodology • Materials • Equipment • Validation data • Supporting documentation (chromatograms, spectra) • Transfer to routine protocol • Reference to SOP
Want to learn more about analytical method validation, FDA and ICH requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links: • ICH, FDA and USP Requirements for Method Validation • How to Validate Analytical Methods and Procedures • Validation of Analytical Methods and Procedures • Eliminate the Confusion - Analytical Method Qualification and Validation • Lifecycle Approach to Analytical Methods with QbD Elements • Analytical Instrument Qualification and System Validation • Lifecycle Approach to Analytical Methods for Drug Products