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Characterization of the trace‐level impurities in the bulk drug citalopram by high‐performance liquid chromatography/tandem multistage mass spectrometry
Author(s) -
Sun Cuirong,
Xu Hui,
Pan Yuanjiang,
Shen Zhiquan,
Wang Danhua
Publication year - 2007
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.3163
Subject(s) - chemistry , chromatography , tandem mass spectrometry , impurity , mass spectrometry , tandem , trace (psycholinguistics) , liquid chromatography–mass spectrometry , characterization (materials science) , analytical chemistry (journal) , nanotechnology , organic chemistry , materials science , composite material , linguistics , philosophy
Five trace impurities were detected in the bulk drug citalopram using high‐performance liquid chromatography with UV detection. A simple and sensitive method suitable for liquid chromatography tandem multistage mass spectrometry (HPLC/MS n ) analysis was developed. Using this method, the fragmentation behavior of citalopram and the impurities was investigated. Four impurities were rapidly characterized, and an unknown impurity was elucidated as 3‐(3‐dimethylaminopropyl)‐ N ‐(1‐(3‐dimethylaminopropyl)‐1‐(4‐fluorophenyl)‐1,3‐dihydroisobenzofuran‐5‐yl)‐3‐(4‐fluorophenyl)‐1,3‐dihydroisobenzofuran‐5‐carboxamide on the basis of the MS n and exact mass evidence, and the proposed structure was further confirmed by nuclear magnetic resonance (NMR) experiments after preparative isolation. Copyright © 2007 John Wiley & Sons, Ltd.