Semi-preparative isolation and structural elucidation of an impurity in citalopram by LC/MS/MS.
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.
Raman
Bhanu
B
Department of Chemistry, K.J. Somaiya College of Science and Commerce, Vidyavihar (E), Mumbai 400077, India. drbhanuraman@rediffmail.com
Sharma
Brajesh A
BA
Ghugare
Pradeep D
PD
Karmuse
Pravin P
PP
Kumar
Ashok
A
D001572:Benzofurans / Q000032:analysis / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D015283:Citalopram / Q000032:analysis / Q000737:chemistry*; D004340:Drug Contamination; D009682:Magnetic Resonance Spectroscopy / Q000379:methods; D017367:Selective Serotonin Reuptake Inhibitors / Q000032:analysis / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013055:Spectrophotometry, Infrared / Q000379:methods
D001572:Benzofurans; D015283:Citalopram; D017367:Selective Serotonin Reuptake Inhibitors; C544698:1-(1,1-bis(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-yl)-4-(dimethylamino)butan-1-one