HPLC Analytical Method Development and Validation

Introduction

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.

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

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

Workshop: Selecting the column and mobile phase
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
Workshop: Validating a typical HPLC method
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

Workshop: Dealing with validation failures and how to avoid failures
End of Day Two: Group discussion and close

The course will include interactive workshops