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Raju, G.
- The Quantitative Determination of Process Related Genotoxic Impurities in Esomeprazole Magnesium by GC-MS
Authors
1 Matrix Laboratoires Ltd., R&D Centre, Jinnaram Mandal, Medak, 502325, IN
2 National Centre for Mass Spectrometry, Indian Institute of Chemical Technology, Hyderabad, 500 007, IN
3 Department of Chemistry, P.G. College of Science, Saifabad, Hyderabad, IN
Source
Asian Journal of Research in Chemistry, Vol 4, No 6 (2011), Pagination: 898-901Abstract
A sensitive Gas chromatography-mass spectrometric (GC-MS) method is developed and validated for the determination of residuals 2-Chloromethyl-4-methoxy-3,5-dimethyl pyridine HCl (2), 2,3,5-Trimethyl pyridine Noxide (3), 4-Nitro-2,3,5-Trimethyl pyridine N-oxide (4) and 4-Methoxy-2,3,5-Trimethyl pyridine N-oxide (5) are genotoxic impurities in Esomeprazole magnesium (1) drug substance. Under the optimal conditions, the recovery for 2, 3, 4, and 5 are between 109.4% to 116.8%, 99.9% to 107.6%, 96.0% to 104.1%, and 87.4% to 105.2% for spiked samples at limits of quantification (LOQ) level in sample preparation. Limits of quantification (LOQ) and detection (LOD) are about 5 ppm and 1.5 ppm for the standard solutions of 2, 3, 4, and 5. The linearity values are 0.9989, 0.9968, 0.9988, and 0.9999 for 2, 3, 4, and 5. Based on these results, the method is applied to determine the residual genotoxic impurities are, 2-Chloro methyl-4-methoxy-3,5-dimethyl pyridine HCl (2), 2,3,5-Trimethyl pyridine Noxide (3), 4-Nitro-2,3,5-Trimethyl pyridine N-oxide (4) and 4-Methoxy-2,3,5-Trimethyl pyridine N-oxide (5) in Esomeprazole magnesium (1) drug substance.
Keywords
Esomeprazole Magnesium, Single Ion Monitoring, Gas Chromatography-Mass Spectrometry.- Validated Chromatographic Method for the Determination of Process Related Genotoxic Impurity in Lansoprazole
Authors
1 Matrix Laboratories Ltd., R&D Centre, Jinnaram, Medak, 502325, IN
2 National Centre for Mass Spectrometry, Indian Institute of Chemical Technology, Hyderabad, IN
3 Department of Chemistry, P.G. College of Science, Saifabad, Hyderabad, IN
Source
Asian Journal of Research in Chemistry, Vol 4, No 6 (2011), Pagination: 965-967Abstract
An LC-MS method for the simultaneous determination of process related impurity of 2-Chloromethyl-3-methyl-4-(2, 2, 2-trifluoroethoxy) pyridine Hydrochloride (CMTP, 1) and RP-LC method for the routine determination of 1 in Lansoprazole (2) was presented. In LC-MS, Hypersil BDS C-18 (150 X 4.6 mm, 5 μm) column was used with mobile phase containing buffer (0.01 M ammonium acetate), acetonitrile, and methanol in 50:45:5 v/v ratios. The flow rate was 0.8 mL min-1 and elution was monitored at 205 nm. LC analysis of 1 was done on Synergi polar RP-80A (250 X 4.6 mm, 4 μm) column using mobile phase containing buffer (0.1% triethyl amine) and acetonitrile in 65:35 v/v ratio. The flow rate was 0.8 mL min-1 and elution was monitored at 205 nm. Both methods were validated as per International Conference on Harmonization (ICH) guidelines. LC-MS is able to quantitate up to 0.9 ppm, whereas with RP-LC up to 30 ppm of 1 could be quantitated.Keywords
Lansoprazole, Column Liquid Chromatography, Liquid Chromatography-Mass Spectrometry.- A Sensitive and Selective GC-MS Method for the Determination of Process Related Genotoxic Impurities in Esomeprazole Magnesium
Authors
1 Matrix Laboratories Ltd., R and D Centre, Jinnaram Mandal, Medak-502325, IN
2 National Centre for Mass Spectrometry, Indian Institute of Chemical Technology, Hyderabad-500007, IN
3 Department of Chemistry, P.G. College of Science, Saifabad, Hyderabad, IN