Current Status and Trends in the Application of Liquid Chromatography (LC and UHPLC) Hyphenated with Tandem Mass Spectrometry for Pharmaceutical Analysis

This Tuesday afternoon session, titled "Current Status and Trends in the Application of Liquid Chromatography (LC and UHPLC) Hyphenated with Tandem Mass Spectrometry for Pharmaceutical Analysis" was presided over by Arindam Roy of Covidien.

The first speaker in the session was John Edwin George of Varian, Inc., with a presentation titled "Tandem MS with Evaporative Light Scattering Detection (ELSD): A Powerful Analytical Combination for the Analysis of Select Pharmaceuticals." He showed the separation of compounds such as cyclodextrins to demonstrate an application of the technique. He noted that ELSD is a universal detection technique that can detect compounds lacking a chromaphore, and that it is compatible with gradient elution and a wide range of solvents.

Yanqun Zhao of Abbott Laboratories then presented a talk titled "Application of LC-MS as an Everyday Tool in the Analytical Process Development of API." She provided a number of real-life examples of the use of LC-MS in a pharmaceutical laboratory. Applications included impurity control in which the technique enabled structure determination; providing information about how the impurity was formed and how it could be eliminated; impurity profiling in the mother liquor; and impurity tracking, and quantitation by LC-MS.

Despite suffering repeated interruptions for equipment repair, Brenda Kesler of Thermo Fisher Scientific exhibited great patience in delivering a talk titled "The LTQ Orbitrap: Defining Its Place in the Drug Development and the Impurity Analysis Workflows." She discussed mass defect filtering; MALDI on the Orbitrap XL mass spectrometer; a study of raclopride, a diagnostic aid for brain disease; and MS-MS at various concentrations and in different matrices.

Robert Ian Ellis of MDS Sciex/Applied Biosystems then presented "Addressing the NEED for SPEED: High Throughput and High Confidence with Novel LC-MS-MS Solutions." His talk focused on how throughput can be improved in a pharmaceutical environment.

After a short recess, Robyn A. Rourick of Kalypsys, Inc. presented a talk titled "The Application of Capillary LC-MS Using Nanospray for the Profiling of Impurities and Degradants." She described methods used in her company for accelerating drug discovery and development. She stressed the need for low detection levels in impurity detection and the use of tailored methods for detecting low-level impurities.

Georges L. Gauthier of Agilent Technologies followed with a presentation titled "Automated Sample Enrichment and High Sensitivity Analysis of DMPK Samples Using HPLC-Chip QQQ MS." He spoke about using a high-capacity enrichment chip-based column for the analysis of pharmaceutical small molecules.

"Realizing the Benefits of Sub-2-Micrometer Particle LC Hyphenated with MS-MS for Pharmaceutical Analysis" was the next talk, presented by Robert S. Plumb of Waters Corporation. He discussed results obtained using LC-MS with sub-2-micrometer column particles in the analysis of the drugs simvastatin and cyclosporine.

The final presentation of the session was given by Min Li of Schering Plough and was titled "Effective Use of LC-MSn Molecular Fingerprinting for the Rapid Structural Identification of Pharmaceutical Impurities." Li presented a case study of the structural determination of betamethazone 17-deoxy-20-hydroxy-21-oic acid diastereomers.