Analytical methods must be validated to provide reliable data for regulatory submissions. These methods are essential for a number of purposes, including testing for QC release, testing of stability samples, testing of reference materials and to provide data to support specifications.
This course provides a comprehensive coverage of the method development and validation requirements that are essential to progress a pharmaceutical compound, at each stage of product development.
Upon completion of this course, delegates will have learned what is necessary to develop and validate methods for drug substance and drug product to comply with international regulatory guidelines.
PROGRAMME
Day One
Analytical method development, part 1
- Theory and factors affecting resolution - a reminder of the importance of resolution, separation factor (selectivity), retention factor (capacity factor) and column efficiency).
- Selecting the HPLC separation mode (reversed-phase, normal-phase etc.)
- Overview of instrumentation
- Selecting the most appropriate detector
- Troubleshooting
Analytical method development, part 2
- Selecting the column for analysis
- Scouting runs as a guide to optimum conditions
- Using chromatographic parameters to decide quality of chromatography
- Gradient/isocratic operation appropriate?
- Selecting and optimising the mobile phase
- The effect of pH, considering pKa of the analyte
End of Day Two: Group discussion
Day Two
Validation of chromatographic methods, part 1
- Introduction to ICH guidelines: ICH Q2(R1)
- Types of analytical procedure to be validated:
- Identification test *Quantitative test (impurities content)
- Limit tests (control of impurities)
- Quantitative test of active moiety (assay vs. external standard)
- A detailed discussion on the parameters to be validated:
- Specificity: peak purity determination (Diode array and MS detectors)
- Linearity
- Range
- Accuracy
- Precision
- Detection Limit
- Quantitation Limit
- Robustness
Validation of chromatographic methods, part 2
- Comparison of the traditional and Quality by Design (QbD) approach to validation
- Extent of validation: how much work at each phase of development?
- Acceptance criteria
- Validation procedures and protocols
- Dealing with validation failures
- Verification of compendial procedures
End of Day Two: Group discussion and close
