Application of LC-NMR to the identification of bulk drug impurities in NK1 antagonist GW597599 (vestipitant).
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.
Molecular Discovery Research, GlaxoSmithKline Medicines Research Centre, Via Fleming 4, 37135 Verona, Italy. stefano.2.provera@gsk.com
Stefano
S
Provera
Giuseppe
G
Guercio
Lucilla
L
Turco
Ornella
O
Curcuruto
Giuseppe
G
Alvaro
Tino
T
Rossi
Carla
C
Marchioro
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004340:Drug Contamination; D004345:Drug Industry / Q000379:methods*; D005464:Fluorobenzenes; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods; D015394:Molecular Structure; D064729:Neurokinin-1 Receptor Antagonists; D010880:Piperidines / Q000032:analysis* / Q000138:chemical synthesis / Q000737:chemistry; D012996:Solutions
D005464:Fluorobenzenes; D064729:Neurokinin-1 Receptor Antagonists; D010880:Piperidines; D012996:Solutions; C534550:vestipitant