Method Validation
Validation Process
The process starts from method definition and development up to reporting of test results. The typical process is as follows:
- Define the application, purpose and scope of the method
- Ensure method development, pre-validation and fine-tuning
- Freeze the method to be validated, develop a validation protocol (specifying validation experiments, acceptance criteria, etc.)
- Execute the validation experiments according to protocol, check that the acceptance criteria were met
- Document the validation results in a validation report
- Approve the method for routine use
- If any changes are needed that go beyond the original validation, ensure additional validation or re-validation
Parameters
Most guidelines require evaluation of the following method validation parameters:
- Precision (Repeatability, Intermediate Precision)
- Accuracy
- Specificity
- Limit of Detection
- Limit of Quantitation
- Linearity and Range
- Robustness (Ruggedness)
- Sensitivity
For more information about the method validation module, see a case study: GC headspace determination of residual solvents in a drug substance, or view software screenshots here.
Related documents
ISO 17025:2005, chapter 5.4.5
ICH Q2(R1)
U.S. FDA, Title 21 of the U.S. CFR: 21 CFR 211—cGMP for finished
pharmaceuticals
U.S. FDA – Guidance for Industry (draft) Analytical Procedures and Methods
Validation: Chemistry, Manufacturing, and Controls and Documentation, 2000
EPA – Method Validation of U.S. Environmental Protection Agency, Microbiological Methods of Analysis
Eurachem – The Fitness for Purpose of Analytical Methods, A Laboratory
Guide to Method Validation and Related Topics, 1998
