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Day 2: TP24
Identification of Drug Metabolites Using NMR and LC-MS-NMR Methods

Titan Z. Gu², Yanli Deng¹ and Neil Spooner
Worldwide Bioanalysis, DMPK ¹ Development DMPK - Upper Merion, DMPK
GlaxoSmithKline Pharmaceuticals, King of Prussia, PA 19406

The recent acquisition of a 700 MHz Bruker NMR magnet along with a LC-NMR-MS system in our laboratory has enabled us to routinely determine metabolite structures in various biological matrices with micrograms of material. Several metabolites of drug GSK-X were isolated by HPLC from rat bile obtained from an isolated perfused rat liver system. No definite structural identification could be obtained due to the presence of endogenous materials in the isolates. Hence, LC-NMR-MS experiment were carried out on the isolates to provide further information on the metabolites of interest. By combining the information of the connectivities among protons, the number of exchangeable protons, the proton chemical shift changes and the MS/MS fragmentation information, the definite structural identifications were readily made. LC-MS-NMR experiment was also carried out on the neat perfused rat bile, and metabolite structures were determined based on one single run of LC-MS-NMR experiment with only 70 mL of neat bile injected.

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