Semi-preparative isolation and structural elucidation of an impurity in citalopram by LC/MS/MS

被引：23

作者：

Raman, Bhanu ^{[1
]}

Sharma, Brajesh A. ^{[1
,2
]}

Ghugare, Pradeep D. ^{[2
]}

Karmuse, Pravin P. ^{[2
]}

Kumar, Ashok ^{[2
]}

机构：

[1] KJ Somaiya Coll Sci & Commerce, Dept Chem, Bombay 400077, Maharashtra, India

[2] Ipca Labs Ltd, Div Chem Res, Mumbai 400067, Maharashtra, India

来源：

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS | 2009年 / 50卷 / 03期

关键词：

Citalopram HBr; Impurities; LC/MS(n); Q-TOF; Semi-preparative HPLC; NMR;

D O I：

10.1016/j.jpba.2009.05.017

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

Two impurities were detected in citalopram bulk drug substance by HPLC analysis. A new LC-ESI/MS method was developed for the identification of impurities. One of the impurities was found to be unknown and has not been reported previously. The structure of the unknown impurity was proposed on the basis of MS(n) data obtained using ion trap mass analyzer and accurate mass obtained using Q-TOF mass analyzer. The impurity was isolated by semi-preparative HPLC. The structure of the impurity was confirmed as 1-(1,1-bis (4-fluorophenyl)-1,3-dihydroisobenzofuran-5-yl)-4-(dimethylamino) butan-1-one hydrobromide by using NMR and IR spectroscopy. (C) 2009 Elsevier B.V. All rights reserved.

引用

页码：377 / 383

页数：7

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