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        Nuclear Magnetic Resonance (NMR)-Based Drug Metabolite Profiling

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        The identification of drug metabolites in biofluids such as urine, plasma and bile is an important step in drug discovery and development. Proton nuclear magnetic resonance (1 H-NMR) spectroscopy can provide detailed information regarding the structural transformation of a compound as a consequence of metabolism. However, successful identification of drug metabolites by 1 H-NMR spectroscopy is generally compromised by the presence of endogenous metabolites, which can obscure the signals of the drug metabolites in question. Hence, sample clean-up and separation of the metabolites from the biofluid matrix is crucial. This is generally achieved by extraction of the biofluid, solid-phase extraction (SPE), high-performance liquid chromatography (HPLC) or any combination of these. Apart from 1 H, other NMR-active nuclei, such as 19 F, can provide a useful handle for metabolite profiling, provided they are not naturally present in the biofluid. Successful studies have shown that the presence of a fluorine-handle on the drug and its metabolites can provide additional qualitative and quantitative data by 19 F-NMR spectroscopy. This chapter provides guidelines and examples of NMR-based drug metabolite profiling.
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