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Application of LC–NMR to the identification of bulk drug impurities in NK1 antagonist GW597599 (vestipitant) |
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| Authors: | Stefano Provera Giuseppe Guercio Lucilla Turco Ornella Curcuruto Giuseppe Alvaro Tino Rossi Carla Marchioro |
| Institution: | 1. Molecular Discovery Research, GlaxoSmithKline Medicines Research Centre, Via Fleming 4, 37135 Verona, Italy;2. Preclinical Drug Discovery, GlaxoSmithKline Medicines Research Centre, Via Fleming 4, 37135 Verona, Italy;3. Neurosciences Centre of Excellence, GlaxoSmithKline Medicines Research Centre, Via Fleming 4, 37135 Verona, Italy |
| Abstract: | Liquid chromatography‐NMR (LC–NMR) spectroscopy was used to obtain detailed information regarding the structure of the major bulk drug impurities present in GW597599 (vestipitant). The one‐dimensional 1H LC–NMR experiments were performed in both continuous and stop‐flow modes on a sample of GW597599 (vestipitant) enriched with mother liquor impurities. The information derived from both LC–NMR and LC–MS data provided the structural information of all major impurities. The full characterisation of the impurities by high‐resolution NMR spectroscopy was ultimately performed on appropriately synthesised compounds. Copyright © 2010 John Wiley & Sons, Ltd. |
| Keywords: | LC– NMR 1H NMR 13C NMR 15N NMR NK1 antagonists vestipitant |