The Chromatography Forum

of Delaware Valley

Abstract:

Country test guidelines for analytical method validations in the Ag industry are discussed, specifically for analysis of technical actives and formulations. Methods are validated under these guidelines and GLP as part of product registrations.  Beyond meeting regulatory guidelines, we also discuss the advantages of improving method precision and accuracy to improve confidence that products meet release specifications.  Finally, a method transfer procedure is discussed which is used to maintain the precision and accuracy of results when the method is transferred to manufacturing labs for product release analyses. 

A wide variety of analytical methods are used in crop protection for the development, process development, reaction monitoring, and quality control of intermediates and finished products.  Techniques include most often HPLC or GC, but also near infrared (NIR), ion chromatography (IC), and others.  There is always a need for precision and accuracy in the methods, but this is particularly true for finished products that are sold to customers.  The methods are used to assure that the product meet specifications.  The industry is highly regulated and the specifications and analytical methods are part of the regulatory approval process.  Validation of the methods to meet regulatory guidelines is challenging, partly due to the various country requirements, but also because the requirements continue to evolve.  Beyond the regulatory requirements are the internal requirements for method capability, i.e. the precision of the method or measurement system relative to the specification range for the product.  A higher method capability gives us more confidence in the correctness of the analyses. 

Transferring a validated and capable method to another laboratory can provide another challenge:  how to maintain the same level of accuracy and precision.  We have used a process successfully for method transfers of assay and impurity methods inside and outside of our company, including 10- to 20-lab international collaborative (CIPAC) studies.  Communication and planning are important to a successful transfer.  It helps to check whether the laboratory has equivalent equipment, method procedures and method qualification requirements are clearly understood, the method set-up is performed correctly, and experiences and best practices are well communicated.  I will describe the test plan that we use and the data evaluation tool that we use for evaluation of the test results and for targeting areas for improvement. 

About the Speaker:

Steve Hansen received his PhD. in Organic Chemistry from the University of Iowa under the guidance of Prof. Donald J. Burton.  The subject of his thesis was the development of synthetic routes to polyfluorinated organic compounds, building small, commercially-available fluorocarbons into larger, functionalized structures.  He began his career with DuPont as a chemist at the Belle Plant, near Charleston, WV, gaining extensive experience in a wide variety of analytical techniques and quality control procedures, including the use of design of experiments for method development.  Currently, he works with FMC Corporation, helping to bring new products to market by developing and transferring methods, conducting GLP studies, and authoring reports used in the registration of those products.  The Operations Analytical group works with expert teams in R&D, including organic chemists, chemical engineers, and registration managers.  This team also works with technical and laboratory experts at manufacturing sites and test facilities, both within FMC and at contract/alliance partners worldwide.