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Method Development and Validation for Quantification of Potential Genotoxic Impurity, PyCl in Lansoprazole Hydrochloride using Liquid Chromatography Combined with Mass Spectrometry
Corresponding Author(s) : K.M.V. Narayana Rao
Asian Journal of Chemistry,
Vol. 33 No. 5 (2021): Vol 33 Issue 5, 2021
Abstract
A sensitive and robust high performance liquid chromatography combined with tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of potential genotoxic impurity (PGI), 2-(chloromethyl)-3-methyl-4-(2,2,2-trifluoroethoxy)-pyridine hydrochloride (PyCl) in lansoprazole as per ICH Q2 guideline. In this method, PyCl and lansoprazole were well-separated from each other on Acquity UPLC BEH-C18 column (50 × 4.6 mm × 1.7 μ) in a gradient elution mode with the mobile phase consisting of 0.1% formic acid in water (mobile phase-A) and acetonitrile (mobile phase-B) at a flow rate of 0.4 mL/min. For the quantitation of Py-Cl, selective ion monitoring (SIM) mode was used with m/z 240 ion in LC-MS method. The validated method was found to be precise, accurate and linear from the range of LOQ level to 150% with respect to sample concentration and the correlation co-efficient was found to be 0.998. Limit of detection (LOD) and limit of quantifications (LOQ) were found to be 0.000012 and 0.000004 mg/mL, respectively. The validated method was found to be sensitive and the recoveries were found to be well within the range from 83.4% to 95.9% for Py-Cl. Further, the solution stability was also established as the same were found to be stable upto 24 h.
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- H.M. Bolt, H. Foth, J.G. Hengstler and G.H. Degen, Toxicol. Lett., 151, 29 (2004); https://doi.org/10.1016/j.toxlet.2004.04.004
- T. McGovern and D. Jacobson-Kram, Trends Analyt. Chem., 25, 790 (2006); https://doi.org/10.1016/j.trac.2006.06.004
- M.A. Cheeseman, E.J. Machuga and A.B. Bailey, Food Chem. Toxicol., 37, 387 (1999); https://doi.org/10.1016/S0278-6915(99)00024-1
- International Conferences on Harmonisation Guideline on Impurities in New Drug Products, Q3B (R2), 25 October (2006).
- Guidelines on the Specification Limits for Residues of Metal Catalysts or Metal Reagents, European Medicines Agency, 21 February (2008).
- European Medicines Agency, Evaluation of Medicines for Human Use, Guideline on the Limits of Genotoxic Impurities.
- R. Kroes, A.G. Renwick, M. Cheeseman, J. Kleiner, I. Mangelsdorf, A. Piersma, B. Schilter, J. Schlatter, F. van Schothorst, J.G. Vos and G. Würtzen, Food Chem. Toxicol., 42, 65 (2004); https://doi.org/10.1016/j.fct.2003.08.006
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- M.A. Raja, S.K. Yadav, A. Rai and S. Mishra, Int. J. Res. Pharm. Sci., 2, 521 (2011).
- P.V. Rao, M.N. Kumar and M.R. Kumar, Sci. Pharm., 81, 183 (2013); https://doi.org/10.3797/scipharm.1210-09
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- D. Stacy, J.D. Connor, N.C. Smallwood and R.A. Lugo, Int. J. Anal. Chem., 2011, 832414 (2011); https://doi.org/10.1155/2011/832414
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- H. Wang, Y. Sun, X. Meng, B. Yang, J. Wang, Y. Yang and J. Gu, J. Sep. Sci., 38, 2960 (2015); https://doi.org/10.1002/jssc.201500462
References
H.M. Bolt, H. Foth, J.G. Hengstler and G.H. Degen, Toxicol. Lett., 151, 29 (2004); https://doi.org/10.1016/j.toxlet.2004.04.004
T. McGovern and D. Jacobson-Kram, Trends Analyt. Chem., 25, 790 (2006); https://doi.org/10.1016/j.trac.2006.06.004
M.A. Cheeseman, E.J. Machuga and A.B. Bailey, Food Chem. Toxicol., 37, 387 (1999); https://doi.org/10.1016/S0278-6915(99)00024-1
International Conferences on Harmonisation Guideline on Impurities in New Drug Products, Q3B (R2), 25 October (2006).
Guidelines on the Specification Limits for Residues of Metal Catalysts or Metal Reagents, European Medicines Agency, 21 February (2008).
European Medicines Agency, Evaluation of Medicines for Human Use, Guideline on the Limits of Genotoxic Impurities.
R. Kroes, A.G. Renwick, M. Cheeseman, J. Kleiner, I. Mangelsdorf, A. Piersma, B. Schilter, J. Schlatter, F. van Schothorst, J.G. Vos and G. Würtzen, Food Chem. Toxicol., 42, 65 (2004); https://doi.org/10.1016/j.fct.2003.08.006
K. Ramakrishna, N.V.V.S.S. Raman, K.M.V.N. Rao, A.V.S.S. Prasad and K.S. Reddy, J. Pharm. Biomed. Anal., 46, 780 (2008); https://doi.org/10.1016/j.jpba.2007.11.013
N. Venugopal, A.V. Bhaskar Reddy, K.G. Reddy, V. Madhavi and G. Madhavi, J. Pharm. Biomed. Anal., 70, 592 (2012); https://doi.org/10.1016/j.jpba.2012.05.031
M. Song, X. Gao, T. Hang and A. Wen, Curr. Ther. Res. Clin. Exp., 70, 228 (2009); https://doi.org/10.1016/j.curtheres.2009.05.002
M.A. Raja, S.K. Yadav, A. Rai and S. Mishra, Int. J. Res. Pharm. Sci., 2, 521 (2011).
P.V. Rao, M.N. Kumar and M.R. Kumar, Sci. Pharm., 81, 183 (2013); https://doi.org/10.3797/scipharm.1210-09
Y. Luo, L. Xu, M. Xu, J. Feng and X. Tang, Asian J. Pharm. Sci., 7, 149 (2012).
D. Stacy, J.D. Connor, N.C. Smallwood and R.A. Lugo, Int. J. Anal. Chem., 2011, 832414 (2011); https://doi.org/10.1155/2011/832414
C.H. Oliveira, R.E. Barrientos-Astigarraga, E. Abib, G.D. Mendes, D.R. da Silva and G. de Nucci, J. Chromatogr. B Analyt. Technol. Biomed. Life Sci., 783, 453 (2003); https://doi.org/10.1016/S1570-0232(02)00711-0
H. Wang, Y. Sun, X. Meng, B. Yang, J. Wang, Y. Yang and J. Gu, J. Sep. Sci., 38, 2960 (2015); https://doi.org/10.1002/jssc.201500462