Molecular Discovery Research, GlaxoSmithKline Medicines Research Centre, Via Fleming 4, 37135 Verona, Italy.
Magn Reson Chem. 2010 Jul;48(7):523-30. doi: 10.1002/mrc.2611.
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 (1)H 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.
液相色谱-核磁共振（LC-NMR）光谱法被用于获得 GW597599（vestipitant）中主要大块药物杂质的结构的详细信息。在含有母液杂质的 GW597599（vestipitant）样品上进行了一维（1）H LC-NMR 实验，分别采用连续和停流模式。从 LC-NMR 和 LC-MS 数据中获得的信息提供了所有主要杂质的结构信息。通过高分辨率 NMR 光谱法对杂质进行了最终的全特征化，所使用的合成物是适当合成的。
