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Current Pharmaceutical Analysis

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ISSN (Print): 1573-4129
ISSN (Online): 1875-676X

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Research Article

Development and Validation of a UPLC-MS/MS Method for the Simultaneous Determination of Verapamil and Trandolapril in Rat Plasma: Application to a Pharmacokinetic Study

Author(s): Subrahmanyam Talari, Anuradha Vejendla* and Ratna Kumari Shetty

Volume 18, Issue 3, 2022

Published on: 02 March, 2021

Page: [291 - 304] Pages: 14

DOI: 10.2174/1573412917666210302145711

Price: $65

Abstract

Background: Verapamil is an excellent drug used for the medication of hypertension and trandolapril. It is an angiotensin-converting-enzyme inhibitor. Hence, it is an interesting method to develop a novel and reliable MS/UPLC strategy for the simultaneous development of verapamil and trandolapril.

Objectives: This research study aims to develop a new, rapid, and sensitive UPLC-MS/MS method for the simultaneous estimation of verapamil and trandolapril in rat plasma using D6- verapamil and D6-trandolapril.

Methods: Separation was carried on column Symmetry C18 column (150x4.6 mm, 3.5 μm) using isocratic elution with a buffer containing 1mL of formic acid in 1L of water and the mixture of two components like Buffer and Acetonitrile in the ratio of 80:20 as mobile phase with 1mL/min flow rate at ambient temperature.

Results: Analysis was performed within 5 minutes over a good linear concentration range from 2.4 ng/mL to 48 ng/mL (r2 = 0.9993 ± 0.018) for verapamil and 10 pg/mL to 200 pg/mL (r2 = 0.9993 ± 0.006) for trandolapril. The extraction recoveries and matrix effect of verapamil and trandolapril were 98.45, 99.95, 98.12, 99.66% and 98.27, 99.89, 97.78, 99.23% respectively, at different QC concentration levels. Precision and recovery study results were determined within the acceptable limit. An electrospray ionization source was used to study verapamil and Trandolapril at m/z 454.72→182.16, 430.25→201.48, and IS for m/z 460.18→ 324.39, 436.28 → 340.52, which were ion pairs of mass analysis. This method has successfully been applied to explore verapamil (1.2 mg/kg) with its internal standard (D6-Verapamil), trandolapril (0.005 mg/kg) with its internal standard (D6-Trandolapril) extracted from rat plasma using liquid-liquid extraction.

Conclusion: This manuscript focuses on the consistent evaluation of the key bioanalytical validation parameters, and the following are discussed: accuracy, precision, sensitivity, selectivity, standard curve, limits of quantification, range, recovery, and stability. These validation parameters are described, together with illustrations of validation methodology applied in the case of chromatographic methods used in bioanalysis.

Keywords: UPLC-MS/MS, verapamil, trandolapril, development, validation, rat plasma.

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[1]
Kesselheim, S. The high cost of prescription drugs in the United States. JAMA, 2016, 316(8), 858-871.
[http://dx.doi.org/10.1001/jama.2016.11237] [PMID: 27552619]
[2]
Everett, N.; Gabra, M. The pharmacology of medieval sedatives: the “Great Rest” of the Antidotarium Nicolai. J. Ethnopharmacol., 2014, 155(1), 443-449.
[http://dx.doi.org/10.1016/j.jep.2014.05.048] [PMID: 24905867]
[3]
Lackland, D.T.; Weber, M.A. Global burden of cardiovascular disease and stroke: hypertension at the core. Can. J. Cardiol., 2015, 31(5), 569-571.
[http://dx.doi.org/10.1016/j.cjca.2015.01.009] [PMID: 25795106]
[4]
DiNicolantonio, J.J.; Mehta, V.; O’Keefe, J.H. Is salt a culprit or an innocent bystander in hypertension, A hypothesis challenging the ancient paradigm. Am. J. Med., 2017, 130(8), 893-899.
[http://dx.doi.org/10.1016/j.amjmed.2017.03.011] [PMID: 28373112]
[5]
Banks, K.; Lo, M.; Khera, A. Angina, in women without obstructive coronary artery disease. Curr. Cardiol. Rev., 2010, 6(1), 71-81.
[http://dx.doi.org/10.2174/157340310790231608] [PMID: 21286281]
[6]
Al-Zaiti, S.S.; Magdic, K.S. Magdic, Paroxysmal supraventricular tachycardia, Pathophysiology, diagnosis and management. Crit. Care Nurs. Clin. North Am., 2016, 28(3), 309-316.
[http://dx.doi.org/10.1016/j.cnc.2016.04.005] [PMID: 27484659]
[7]
Lau, E.W.; Ng, G.A. Comparison of the performance of three diagnostic algorithms for regular broad complex tachycardia in practical application. Pacing Clin. Electrophysiol., 2002, 25(5), 822-827.
[http://dx.doi.org/10.1046/j.1460-9592.2002.00822.x] [PMID: 12049375]
[8]
Rajapakse, T.; Pringsheim, T. Nutraceuticals in migraine, A summary of existing guidelines for use. Headache, 2016, 56(4), 808-816.
[http://dx.doi.org/10.1111/head.12789] [PMID: 26954394]
[9]
Paine, M.; Lulli, P.; Farinelli, I.; Simeoni, S.; De Filippis, S.; Patacchioli, F.R.; Martelletti, P. Genetics of migraine and pharmacogenomics, some considerations. The journal of head and pain,, 2007, 8(6), 334-9.
[10]
Tfelt-Hansen, P.C.; Jensen, R.H. Management of cluster headache. CNS Drugs, 2012, 26(7), 571-580.
[http://dx.doi.org/10.2165/11632850-000000000-00000] [PMID: 22650381]
[11]
Merison, K.; Jacobs, H. Diagnosis and treatment of childhood migraine. Curr. Treat. Options Neurol., 2016, 18(11), 48.
[http://dx.doi.org/10.1007/s11940-016-0431-4] [PMID: 27704257]
[12]
Kienle, A.; Lilge, L.; Vitkin, I.A.; Patterson, M.S.; Wilson, B.C.; Hibst, R.; Steiner, R. Why do veins appear blue? A new look at an old question. Appl. Opt., 1996, 35(7), 1151.
[http://dx.doi.org/10.1364/AO.35.001151] [PMID: 21085227]
[13]
Hylands, M.; Moller, M.H.; Asfar, P.; Toma, A.; Frenette, A.J.; Beaudoin, N.; Belley-Côté, É.; D’Aragon, F.; Laake, J.H.; Siemieniuk, R.A.; Charbonney, E.; Lauzier, F.; Kwong, J.; Rochwerg, B.; Vandvik, P.O.; Guyatt, G.; Lamontagne, F. A systematic review of vasopressor blood pressure targets in critically ill adults with hypotension. Can. J. Anaesth., 2017, 64(7), 703-715.
[http://dx.doi.org/10.1007/s12630-017-0877-1] [PMID: 28497426]
[14]
Anwar, Rakshit Untreated relative hypotension measured as Perfusion pressure deficit during management of shock and new onset acute kidney injury-A literature review. Shock, Ovid technologies, 2018, 49(5), 497-507.
[15]
Helena Britt, S. Fahridin, Presentations of nausea and vomiting. Aust. Fam. Physician, 2007, 36(9), 673-784.
[16]
Tramer, M.R.; Carroll, D.; Campbell, F.A; Reynolds, D.J.; Moore, R.A.; McQuay, H.J. Cannabinoids for control of chemotherapy induced nausea and vomiting. Quantitative systematic review,, 2001, 323(7303), 16-21.
[17]
Brenner, D.M.; Shah, M. Chronic Constipation. Gastroenterol. Clin. North Am., 2016, 45(2), 205-216.
[http://dx.doi.org/10.1016/j.gtc.2016.02.013] [PMID: 27261894]
[18]
Andromanakos, N.; Skandalakis, P.; Troupis, T.; Filippou, D. Constipation of anorectal outlet obstruction: pathophysiology, evaluation and management. J. Gastroenterol. Hepatol., 2006, 21(4), 638-646.
[http://dx.doi.org/10.1111/j.1440-1746.2006.04333.x] [PMID: 16677147]
[19]
Thomsen, S.F. Atopic dermatitis natural history, diagnosis and treatments allergy., 2014, 1-7.
[20]
Kuck, K.H.; Bordachar, P.; Borggrefe, M.; Boriani, G.; Burri, H.; Leyva, F.; Schauerte, P.; Theuns, D.; Thibault, B.; Kirchhof, P.; Hasenfuss, G.; Dickstein, K.; Leclercq, C.; Linde, C.; Tavazzi, L.; Ruschitzka, F. Leyva, Fet al, New devices in heart failure, A European heart rhythm association report developed by the European heart rhythm association, endorsed by the heart failure association. Europace, 2014, 16(1), 109-128.
[http://dx.doi.org/10.1093/europace/eut311] [PMID: 24265466]
[21]
Metra, M.; Teerlink, J.R. Heart failure. Lancet, 2017, 390(10106), 1981-1995.
[http://dx.doi.org/10.1016/S0140-6736(17)31071-1] [PMID: 28460827]
[22]
Wang, X.; Wang, G.; Lemos, J.R.; Treistman, S.N. Ethanol directly modulates gating of a dihydropyridine-sensitive Ca2+ channel in neurohypophysial terminals. J. Neurosci., 1994, 14(9), 5453-5460.
[http://dx.doi.org/10.1523/JNEUROSCI.14-09-05453.1994] [PMID: 7521910]
[23]
Sidorenkov, G.; Navis, G. Safety of ACE inhibitor therapies in patients with chronic kidney disease. Expert Opin. Drug Saf., 2014, 13(10), 1383-1395.
[http://dx.doi.org/10.1517/14740338.2014.951328] [PMID: 25148900]
[24]
Rogers, J.M.; Kavlock, R.J. Developmental toxicology.Casarett and Doulls toxicology; Klaassen, C.D., Ed.; , 1996, pp. 301-331.
[25]
Hemming, M.L.; Selkoe, D.J. Amyloid beta protein is degraded by cellular angiotensin converting enzyme and elevated by an ACE inhibitor. J. Biol. Chem., 2005, 280(45), 37644-50.
[26]
Wang, W.; McKinnie, S.M.; Farhan, M.; Paul, M.; McDonald, T.; McLean, B.; Llorens-Cortes, C.; Hazra, S.; Murray, A.G.; Vederas, J.C.; Oudit, G.Y. Angiotensin converting enzyme 2 metabolizes and partially inactivates pyrapelin-13 and Apelin-17. Physiological effects in the cardiovascular system. Hypertension, 2016, 68(2), 365-377.
[http://dx.doi.org/10.1161/HYPERTENSIONAHA.115.06892] [PMID: 27217402]
[27]
Nguyen, G. Renin, (pro)renin and receptor: an update. Clin. Sci. (Lond.), 2011, 120(5), 169-178.
[http://dx.doi.org/10.1042/CS20100432] [PMID: 21087212]
[28]
Gradman, A.H.; Schmieder, R.E.; Lins, R.L.; Nussberger, J.; Chiang, Y.; Bedigian, M.P. Aliskiren, a novel orally effective renin inhibitor, provides dose-dependent antihypertensive efficacy and placebo-like tolerability in hypertensive patients. Circulation, 2005, 111(8), 1012-1018.
[http://dx.doi.org/10.1161/01.CIR.0000156466.02908.ED] [PMID: 15723979]
[29]
Bioanalytical method validation guidance for industry. U.S. Department of Health and Human services Food and drug administration. Biopharmaceutics, 2018.www.fda.gov/files/drugs/published/Bioanalytical-Method-Validation-Guidance-for-Industry.pdf
[30]
Compendium of CPCSEA. Guidelines on the regulation of scientific experiments on animals., 2007.49-96.www.cpcsea.nic.in
[31]
Luke Brewer, K.; Jace Jones, W.; Blackwood, B. Mariette Barbier, Amanda Oglesby Sherrrouse and A Maureen Kane. Development and bio analytical method validation of an LC-MS/MS assay for simultaneous quantitation of 2-alkyl-4(1H)-quinolones for application in bacteria cell culture and lung tissues. Anal. Bioanal. Chem., 2020, 412, 1521-1534.
[http://dx.doi.org/10.1007/s00216-019-02374-0] [PMID: 31993728]
[32]
Wichitnithad, W.; Nantaphol, S.; Vicheantawatchai, P.; Kiatkumjorn, T.; Wangkangwan, W.; Rojsitthisak, P. Development and validation of liquid chromatography-tandem mass spectrometry method for simple analysis of sumatriptan and its application in bioequivalence study. Pharmaceuticals (Basel), 2020, 13(2), 21.
[http://dx.doi.org/10.3390/ph13020021]
[33]
Monica, W.; Ammerman, J.; Lisio, P.D.; Killmer, J.; Kyle, D.; Mainstone, E.; Porter, L.; Zhang, T. LC-MS/MS Bioanalysis method development, validation and sample analysis: Points to consider when conducting nonclinical and clinical studies in accordance with current regulatory guidances. J. Anal. Bioanal. Tech., 2011, S4.
[34]
Kanala, K.; T; Hwisa, N.; Chandu, B.R.; Katakam, P.; Khagga, M.; Challa, B.R.; Khagga, B. Bioanalytical method development and validation of milnacipran in rat plasma by LC-MS/MS detection and its application to a pharmacokinetic study. J. Pharm. Anal., 2013, 3(6), 481-488.
[http://dx.doi.org/10.1016/j.jpha.2013.03.009] [PMID: 29403859]
[35]
Kaza, M.; Karaźniewicz-Łada, M.; Kosicka, K.; Siemiątkowska, A.; Rudzki, P.J. Bioanalytical method validation: new FDA guidance vs. EMA guideline. Better or worse? J. Pharm. Biomed. Anal., 2019, 165, 381-385.
[http://dx.doi.org/10.1016/j.jpba.2018.12.030] [PMID: 30590335]
[36]
Nuland, M.V.; Rosing, H.; Schellens, J.H.M.; Beijnen, J.H. Bio analytical LC-MS/MS validation of therapeutic drug monitoring assay in oncology. Biomed. Chromatogr., 2019, 4623.
[PMID: 31215049]
[37]
Jenkins, R.; Duggan, J.X.; Aubry, A.F.; Zeng, J.; Lee, J.W.; Cojocaru, L.; Dufield, D.; Garofolo, F.; Kaur, S.; Schultz, G.A.; Xu, K.; Yang, Z.; Yu, J.; Zhang, Y.J.; Vazvaei, F. Recommendations for validation of LC-MS/MS bioanalytical methods for protein biotherapeutics. AAPS J., 2015, 17(1), 1-16.
[http://dx.doi.org/10.1208/s12248-014-9685-5] [PMID: 25392238]
[38]
Ravi Kumar, K.; Challa, B.R.; Chandu, B.R.; Chandrasekhar, K.B. Bio analytical method development and validation of Memantine in Human plasma by high performance liquid chromatography with tandem mass spectrometry: Application to bio equivalence study. J. Anal. Methods Chem., 2012.101249
[39]
Singh, B.; Sharma, S.; Dubey, N.; Dwivedi, A.; Lokhandae, R.S. Bioanalytical method development and validation of alimemazine in human plasma by LC-MS/MS and its application in bioequivalence studies. J. Pharm. Bioallied Sci., 2013, 5(4), 257-264.
[http://dx.doi.org/10.4103/0975-7406.120068] [PMID: 24302833]
[40]
Jemal, M.; Ouyang, Z.; Xia, Y.Q. Systematic LC-MS/MS bioanalytical method development that incorporates plasma phospholipids risk avoidance, usage of incurred sample and well thought-out chromatography. Biomed. Chromatogr. 2010, 24(1), 2-19.
[http://dx.doi.org/10.1002/bmc.1373] [PMID: 20017121]
[41]
van Nuland, M.; Rosing, H.; Schellens, J.H.M.; Beijnen, J.H. Bioanalytical LC-MS/MS validation of therapeutic drug monitoring assays in oncology. Biomed. Chromatogr., 2020, 34(1)e4623
[http://dx.doi.org/10.1002/bmc.4623] [PMID: 31215049]

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