title: Method development and validation study for quantitative determination of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride a genotoxic impurity in pantoprazole active pharmaceutical ingredient (API) by LC/MS/MS.
abstract: A sensitive and selective liquid chromatographic-tandem mass spectrometric (LC/MS/MS) method was developed and validated for the trace analysis (>1 ppm level) of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride a genotoxic impurity in pantoprazole sodium drug substances. LC/MS/MS analysis of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride was done on Hypersil BDS C18 (50 mm × 4.6 mm) 3 μm column and 10 mM ammonium acetate in 1000 mL of water was used as buffer. The mobile phase used was in the ratio of buffer-acetonitrile (79:21, v/v). The flow rate was 1.0 mL/min and elution was monitored at 210 nm. The method was validated as per International Conference on Harmonization (ICH) guidelines. LC/MS/MS is able to quantitate up to 0.3 ppm of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride.
authors: Department of Chemistry, Sri Venkateswara University, Tirupati, AP 517502, India.
authors: N
authors: N
authors: Venugopal
authors: A Vijaya
authors: AV
authors: Bhaskar Reddy
authors: K
authors: K
authors: Gangadhar Reddy
authors: V
authors: V
authors: Madhavi
authors: G
authors: G
authors: Madhavi
mesh_terms: D053799:2-Pyridinylmethylsulfinylbenzimidazoles / Q000032:analysis*; D000085:Acetates / Q000737:chemistry; D000097:Acetonitriles / Q000737:chemistry; D002021:Buffers; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000592:standards; D004340:Drug Contamination; D057230:Limit of Detection; D016014:Linear Models; D009153:Mutagens / Q000032:analysis*; D000077402:Pantoprazole; D054328:Proton Pump Inhibitors / Q000032:analysis*; D011725:Pyridines; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry / Q000592:standards
chemical_list: D053799:2-Pyridinylmethylsulfinylbenzimidazoles; C578073:2-chloromethyl-3,4-dimethoxypyridine; D000085:Acetates; D000097:Acetonitriles; D002021:Buffers; D009153:Mutagens; D054328:Proton Pump Inhibitors; D011725:Pyridines; D000077402:Pantoprazole; C018824:ammonium acetate; C032159:acetonitrile