HPLC Analytical Method Development and Validation

Overview

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.

Who Should Attend?

Scientists working with HPLC who need to further their understanding of the technique in order to develop better methods faster. Scientists who have to validate HPLC methods in accordance with current internationally-accepted guidance. HPLC technicians working in R&D laboratories, quality control laboratories and stability testing laboratories.

Managers with a responsibility for generating regulatory submissions.

Course 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

Workshop: Selecting the separation mode

Analytical method development, part 2

• Gradient/isocratic operation appropriate?
• Selecting the column for analysis
• Selecting and optimising the mobile phase
• The effect of pH, considering pKa of the analyte

Workshop: Selecting the column and mobile phase

End of Day One: Group discussion

Day Two

Developing stability-indicating methods

• Requirements for a stability-indicating analytical method
• Anticipation of likely degradation products * From experience with compound * From forced degradation (stress testing) of drug substance, as per ICH guidance * Note findings of stress-testing industry comparison * Are degradation products likely to be enantiomers or diastereoisomers?
• Calculation of mass balance and its significance

Workshop: Developing stability-indicating methods

Validation of chromatographic methods, part 1

• Introduction to ICH guidelines: ICH Q2(R1)
• 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

• Extent of validation: how much work at each phase of development?
• Acceptance criteria
• Validation procedures and protocols
• Dealing with validation failures

Workshop: Validation of chromatographic methods

End of Day Two: Group discussion and close

The course will include interactive workshops