E17: How to Develop Validated HPLC Methods: Rational Design with Practical Statistics & Troubleshooting

Two-Day Course 

Dr. Brian A. Bidlingmeyer, Analytical Acumen Inc., Wilmington, DE
Dr. Stanley N. Deming, Statistical Designs, Houston, TX

This two-day course offers practical training for the practicing scientist. This course takes the participant step-by-step through the concepts, techniques and tools necessary to develop validated HPLC methods. Learn a rapid, systematic approach to HPLC methods development that provides sustainable validation by using statistical process control (SPC) tools. Rather than developing the HPLC method and then validating it, this course proposes following a streamlined, iterative process to integrate the method development and validation activities. The approach is effective, efficient and productive. The emphasis is on practical issues associated with developing validated HPLC methods. Case studies illustrate specific problems and how to approach them, how to carry out routine maintenance to prevent loss of validation, and how to set diagnostics to recognize behavior that requires troubleshooting. Discuss your specific method development/validation problems with instructors who have more than 60 years of combined experience in industry and academe. You will leave with a firm strategy for developing your own continually validated HPLC methods.

This two-day course is intended for individuals who will be or are developing and/or doing quantitative PLC analyses. Laboratory managers, supervisors, analysts, chemists, biologists, engineers and technicians who are responsible for the continual use of validated high- performance liquid chromatographic methods of chemical analysis should attend this course. Those working in R&D, manufacturing, QA/QC, methods development, process development, product testing, pharmaceuticals, biotechnology, organic chemicals, petroleum, environmental, foods, flavors, fragrances, pesticides, testing services laboratories, and occupational health and safety testing will all benefit from this course.

1. Method Evolution
     * Thinking ahead makes the tasks easier
     * The top four items to be successful
2. Basic Statistical Concepts
     * Calculations with statistical significance
     * Parameters of merit
3. Detection Options
     * Choices and trade-offs
     * Typical uses and sensitivities
4. Determining Accuracy, Precision and Linearity
     * Making measurements
     * Proper calculation of validation parameters
5. Achieving Separations
     * The chemistry of resolution
     * Follow the flow chart: a rational strategy for achieving resolution
6. Sample Preparation
     * Review of techniques
     * How to improve the analysis
7. Determining LOD, LOQ, MDL
     * Understanding your limits
     * A simple, fundamental statistical approach
8. Achieving Method Stability and Robustness
     * System suitability
     * System component contributions
9. Optimizing Using Window Diagrams
     * Finding the tallest trees in the forest
     * Choosing the best of several optima
10. Using Statistical Quality Control of Separations
     * An easy graphical method
     * Achieving sustainable validation
11. Troubleshooting Out-of-control Systems
     * Things you often forget to look for
     * Group discussion of typical issues
12. Putting It All Together
     * Approaching the steps to validating a method
     * When steps are necessary and when they’re not
13. Case Studies

Dr. Brian A. Bidlingmeyer is employed by Agilent Technologies in Wilmington, DE. He is an accomplished separation scientist who has work experience in the chemical, pharmaceutical and instrumentation industries. He has published 2 books and more than 80 papers. Brian is the Chairman-elect of the Separations Science Subdivision of the American Chemical Society’s Analytical Division and is active in the ASTM committee concerning chromatographic practices. He has made significant contributions to the practice and understanding of modern HPLC and has received numerous awards including the Heinrich Emmanual Merck Prize for contributions to analytical chemistry, the International Ion Chromatography Award for contributions to that area, and an IR 100 Award for a new method for amino acid analysis (Pico Tag Method). He is presently an associate editor of the Journal of Chromatographic Science.

Dr. Stanley N. Deming is Professor Emeritus at the University of Houston in Houston, TX. He is also the President of Statistical Designs, a firm that offers short courses and consulting in the areas of methods development, process optimization, statistical experimental design, and the statistical analysis of laboratory data. He has taught (with Dr. Stephen L. Morgan and Dr. Brian A. Bidlingmeyer) more than 650 highly acclaimed short courses for the ACS and other organizations. He has co-authored more than 100 papers and four books, including most recently The 4PL: A Guide to the Use of the Four-Parameter Logistic Model in Bioassay. He has been a member of the editorial boards of <Critical Reviews in Analytical Chemistry>, the Journal of Chemometrics, and Chemometrics and Intelligent Laboratory Systems. He currently writes a statistics column for American Laboratory.