Workshop/conference report—Quantitative bioanalytical methods validation and implementation: Best practices for chromatographic and ligand binding assays

Conclusion

For quantitative bioanalytical method validation procedure and requirements, there was a relatively good agreement between chromatographic assays and ligand-binding assays. It was realized that the quantitative and qualitative aspects of bioanalytical method validation should be reviewed and applied appropriately.

• 1. Some of the major concerns between the 2 methodologies related to the acceptable total error for precision and accuracy determination and acceptance criteria for an analytical run. The acceptable total error for precision and accuracy for both the methodologies is less than 30. The 4–6–15 rule for accepting an analytical run by a chromatographic method remained acceptable while a 4–6–20 rule was recommended for ligand-binding methodology.

• 2. The 3rd AAPS/FDA Bioanalytical Workshop clarified the issues related to placement of QC samples, determination of matrix effect, stability considerations, use of internal standards, and system suitability tests.

• 3. There was a major concern and issues raised with respect to stability and reproducibility of incurred samples. This should be addressed for all analytical methods employed. It was left to the investigators to use their scientific judgment to address the issue.

• 4. In general, the 3rd AAPS/FDA Bioanalytical Workshop provided a forum to discuss and clarify regulatory concerns regarding bioanalytical method validation issues.