Asian Journal of Research in Chemistry

M. Yogeshwar Reddy ¹, V. Ramesh ², Ch. Kista Reddy ³, N. Venugopal ¹, G. Saravanana ¹, M. V. Suryanarayana ¹, B. Shyam Sunder ¹, R. Surendranath Reddy ¹, G. Raju ²

Affiliations
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

Abstract

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.

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M. Yogeshwar Reddy ¹, V. Ramesh ², Ch. Kista Reddy ³, N. Venugopal ¹, G. Saravanana ¹, M. V. Suryanarayana ¹, B. Shyam Sunder ¹, R. Surendranath Reddy ¹, G. Raju ²

Affiliations
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

Abstract

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.

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M. Yogeshwar Reddy ¹, V. Ramesh ², Ch. Kista Reddy ³, M. V. Suryanarayana ¹, M. Dilip Kumar ¹, G. Raju ², G. Saravanan ¹, Debashish Datta ¹

Affiliations
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

Abstract

A sensitive gas chromatography (GC)-mass spectrometry (MS) method is developed and validated for the determination of the residues p-Anisidine and 4-Methoxy-2-nitro aniline as genotoxic impurities in Esomeprazole magnesium drug substance.

Keywords

GC-MS, Esomeprazole, Selected Ion Monitoring.

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M. Yogeshwar Reddy ¹, V. Ramesh ², Ch. Kista Reddy ³, N. Venugopal ¹, G. Saravanan ¹, Y. Suresh ¹, M. Suryanarayana ¹, Debashish Datta ¹, B. Raju ²

Affiliations
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

Abstract

A Liquid chromatographic (LC) method using mass spectrometric (MS) detection was developed and validated for the trace analysis (ppm level) of 4-Bromo methyl-2'-Cyanobiphenyl in Valsartan drug substances. LC analysis of 4-Bromo methyl-2'-Cyanobiphenyl was done on Necleosil C18 (100 mm×4.6 mm, 3 μm) column and the mobile phase is in the ratio of 50:50:1 containing water, acetonitrile, and acetic acid. The flow rate was 1.0 mL min^-1 and the elution was monitored at 225 nm. The method was validated as per International Conference on Harmonization (ICH) guidelines. LC-MS is able to quantitate up to 1.0 ppm of 4-Bromo methyl-2'-cyanobiphenyl.

Keywords

Liquid Chromatography, Mass Spectrometry Valsartan.

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