Frequent mistakes made during method validation-a retrospective study.
Insufficient robustness of studies
Robustness studies should be planned with a scientifically sound method which depends on test sample specification. To be sure the sample meets particular specifications; the methodology must be tested against different parameters. A good example could be:
- No testing the column enough during analytical validation studies.
- Assure that each column is assigned to a particular project. Provide clear guidance for column cleaning and storage.
Insufficient acceptance criteria
Improper use of specifications which does not incorporate critical quality attributes. A wide or inaccurate sample acceptance criteria will probably produce in obtaining inaccurate sample results.
Lack of filter study for standard or sample solutions
In most of method validations, filter study is not conducted. Regardless of whether the solution is clear and free from any particulate matter, a filter study should be conducted during method validation studies.
Other points to be considered
- Inefficient or failure to include documentations for deviations or investigations. Capture all activities in the report, along with any deviation, justification and amendment.
- Method validation should be peer reviewed and approved by QA.
- Clearly note all critical findings from the forced degradation and validation studies. Failure for the analytical methods to demonstrate stability.
- It is crucial that the limit of LOD and LOQ be captured in the method for accurate sample results reporting.
- For method transfer, obtain feedback from the receiving lab(QC lab) and incorporate these comments and observations in the method.
- For method transfer and validations, quality assurance department should conduct an Annual review of the method, and collect feedback from analyst and incorporate those changes accordingly. (updated on 10.10.2020)
