A rapid and efficient approach to metabolite identification using nuclear magnetic resonance spectroscopy, liquid chromatography/mass spectrometry and liquid chromatography/nuclear magnetic resonance spectroscopy/sequential mass spectrometry

Abstract

High‐performance liquid chromatography, nuclear magnetic resonance (NMR) spectroscopy and sequential mass spectrometry (MSn) have been combined to allow rapid and effective identification of metabolites in urine following administration of the novel non‐nucleoside reverse transcriptase inhibitor, GW420867. The combination of these techniques has enabled structural and molecular weight information to be interpreted by the analyst with greater efficiency and accuracy. This work demonstrates the potential of coupling MSn using an ion trap spectrometer with NMR spectroscopy, providing an extremely powerful technique for structural elucidation. Copyright © 1998 John Wiley & Sons, Ltd.

Use of monolithic silica columns to increase analytical throughput for metabolite identification by liquid chromatography/tandem mass spectrometry

“…1) can be separated sufficiently in under a minute, allowing both MS and MS/MS spectra to be acquired. Previous work has demonstrated the application of data‐dependent MS/MS (auto MS/MS) using the Esquire ion trap for the purpose of metabolite identification 1,. 11 Although this feature has proved extremely useful, it was not possible in this instance due to the narrow peak widths observed using the silica ‘rod’ column.…”

“…The identification of drug metabolites in biological fluids is an essential part of the drug discovery and development process. This function is usually accomplished by the use of high‐resolution liquid chromatography coupled to mass spectrometry (MS) and/or nuclear magnetic resonance (NMR) spectroscopy 1. In order to achieve sufficient resolution of metabolites and endogenous components, high‐resolution columns (10–25 cm in length), together with reversed‐phase gradient elution over 20–30 min, is usually required.…”

Metabolomic Fingerprinting: Challenges and Opportunities

“…Until that point, LC-MS, either alone 100 or in conjunction 101 with other techniques, can be used to identify unknown metabolites.…”

LC‐NMR Overview and Pharmaceutical Applications

“…In the area of natural products, this technique has been applied as a rapid screening method of searching unknown marine natural products in chromatographic fractions [108] and for the separation and characterization of natural products from plant origin [109,110]. In the field of drug metabolism, LC-MS-NMR has been extensively applied for the identification of metabolites [112][113][114][115][116][117][118][119][120]. In the field of drug metabolism, LC-MS-NMR has been extensively applied for the identification of metabolites [112][113][114][115][116][117][118][119][120].…”