UV Spectrophotometric Method Development and Validation for the Simultaneous Estimation of Antihypertensive Drugs
DOI:
https://doi.org/10.63682/jns.v13i1.9592Keywords:
Olmesartan Medoxomil, Sacubitril Calcium, FTIR, DSC, UV Spectrophotometry, Method Validation, Antihypertensive Drugs, ICH GuidelinesAbstract
The present study focuses on the analytical characterization and UV spectrophotometric method validation for two widely used antihypertensive drugs, Olmesartan Medoxomil and Sacubitril Calcium. FTIR spectroscopy confirmed the presence of functional groups such as –OH, C=O, and aromatic rings, indicating the structural integrity of both compounds. DSC analysis revealed sharp melting endotherms at 177.18°C for Olmesartan Medoxomil and 156.96°C for Sacubitril Calcium, confirming their thermal stability and purity. UV spectrophotometric analysis was performed to determine the λmax, which was found to be 255 nm for Olmesartan Medoxomil and 254 nm for Sacubitril Calcium. The method was validated as per ICH guidelines and showed excellent linearity, with correlation coefficients (R²) of 0.9996 and 0.9995 respectively. Accuracy studies revealed percent recoveries close to 100%, while precision, robustness, and ruggedness assessments confirmed method reliability. The low LOD and LOQ values indicate good sensitivity. Overall, the developed method is simple, rapid, precise, and suitable for routine quality control of both drugs in pharmaceutical formulations.
Downloads
References
British Pharmacopoeia. London: Medicines and Healthcare products Regulatory Agency; 2007. Vol. 2, p. 1078–80, 1609–11.
United States Pharmacopoeia 41, National Formulary 36. Validation of Compendial Methods. Rockville (MD): United States Pharmacopeial Convention; 2018. p. 2139, 3240.
European Pharmacopoeia. 9th ed. Strasbourg: Council of Europe; 2019. p. 2755, 3296.
Erk N. Comparison of spectrophotometric and an LC method for the determination of perindopril and indapamide in pharmaceutical formulations. J Pharm Biomed Anal. 2001;26(1):43–52.
Maczka P, Gumieniczek A, Galeza J, Pietras R. Zero crossing and ratio spectra derivative spectrophotometry for the dissolution tests of amlodipine and perindopril in their fixed dose formulations. Curr Issues Pharm Med Sci. 2014;27(2):113–7.
Modi DK, Patel CN. Development and validation of spectrophotometric method for simultaneous estimation of perindopril and indapamide in combined dosage form by simultaneous equation method. Eurasian J Anal Chem. 2011;6(1):46–52.
Jogia H, Khandelwal U, Gandhi T, Singh S, Modi D. Development and validation of a stability-indicating assay method for simultaneous determination of perindopril and indapamide in combined dosage form by reversed-phase high performance liquid chromatography. J AOAC Int. 2010;93(1):108–15.
Szabo ZI, Reti ZZ, Gagyi L, Kis EL, Sipos E. Simultaneous quantification of related substances of perindopril tert-butylamine using a novel stability-indicating liquid chromatographic method. J Chromatogr Sci. 2015;53:424–30.
Bhoir V, Hibare V, Damle MC. Development and validation of stability-indicating HPTLC method for the estimation of perindopril and indapamide. Int J Pharm Pharm Sci. 2014;6(7):621–5.
Campbell DB. The possible mode of action of indapamide: a review. Curr Med Res Opin. 1983;8:9–24.
Pai JB, Shetty SK, Chenna GP, Gopinath B, Manzoor A. Development of new spectrophotometric methods for the determination of indapamide in bulk and pharmaceutical formulations. Int J ChemTech Res. 2011;3(2):755–60.
Gupta Y, Shrivastava A, Duggal D, Patel A, Agrawal S. A new RP-HPLC method for simultaneous estimation of nebivolol hydrochloride and hydrochlorothiazide in dosage forms. J Young Pharm. 2009;1(3):264–9.
Joshi HS, Kher GJ, Ram VR, Dodiya BL. HPLC method development and validation of combined dosage form of atenolol and indapamide in tablets. Int J PharmTech Res. 2011;3(3):3277–98.
Shah DA, Bhatt KK, Mehta RS, Baldania SL, Gandhi TR. Stability indicating RP-HPLC estimation of nebivolol hydrochloride in pharmaceutical formulations. Indian J Pharm Sci. 2008;70(5):591–5.
Pawar PV, Gaikwad PD, Bankar VH, Pawar SP. Development and validation of RP-HPLC method for simultaneous estimation of atenolol and indapamide in pharmaceutical dosage form. Int J Res Ayurveda Pharm. 2011;2(3):918–23.
Doshi AS, Bhagwan SS, Mehta TN, Gupta VK, Gunta S. Determination of nebivolol and valsartan in a fixed-dose combination by liquid chromatography. J AOAC Int. 2008;91(2):292–8.
Sahoo MK, Giri RK, Barik CS, Kanungo SK, Ravi Kumar BVV. RP-HPLC method for the estimation of nebivolol in tablet dosage form. E-J Chem. 2009;6(3):915–9.
Patel AR, Chandrul KK. Method development, validation and stability study for simultaneous estimation of telmisartan and indapamide by reverse phase-high performance liquid chromatography in pure and marketed formulation. Int J Pharm Biomed Res. 2011;2(1):4–16.
Al Masud A, Rahman MM, Hasan M, Ripon MKH, Khan AR, Islam MR, et al. Validated spectrophotometric method for estimation of Olmesartan Medoxomil in pharmaceutical formulation. Int J Pharm Life Sci. 2012;1(3):1–6.
Sharma T, Moitra SK, Si SC, Gowrisankar D. Visible spectrophotometric determination of Olmesartan Medoxomil in pharmaceutical formulations. Asian J Chem. 2012;24(8):3771–2.
Hemke AT, Bhure MV, Chouhan KS, Gupta KR, Wadodkar SG. UV spectrophotometric determination of Hydrochlorothiazide and Olmesartan Medoxomil in pharmaceutical formulation. J Chem. 2010;2010:826585.
Vicent L, Esteban-Fernández A, Gómez-Bueno M, De-Juan J, Díez-Villanueva P, Iniesta ÁM, et al. Sacubitril/Valsartan in daily clinical practice: data from a prospective registry. J Cardiovasc Pharmacol. 2019;73(2):118–24.
Sharma RN, Pancholi SS, Sawale V, Dhabarde DM, Mahapatra DK. Development and validation of UV spectrophotometric method for simultaneous estimation of Olmesartan Medoxomil and Chlorthalidone in bulk and tablet. Eurasian J Anal Chem. 2017;12(1):1–6.
Vora BN, Parmar RR, Nayak PP, Shah DA. Development and validation of the simultaneous UV spectrophotometric method for estimation of metoprolol succinate and Olmesartan Medoxomil in the tablet dosage form. Pharm Methods. 2012;3(1):44–7.
Ghelani NC, Bhalodiya K, Dadhania K, Faldu S. Development and validation of spectrophotometric method for simultaneous estimation of Olmesartan Medoxomil and Cilnidipine by simultaneous equation method. PharmaTutor. 2014;2(4):1–6.
Pandiya H, Rathore KS. UV spectrophotometric determination of Olmesartan Medoxomil in pure and pharmaceutical formulation. PharmaTutor. 2019;Aug:1–6.
Celebier M, Altinoz S. Determination of Olmesartan Medoxomil in tablets by UV–Vis spectrophotometry. Pharmazie. 2007;62(6):419–22.
Gu J, Noe A, Chandra P, Al-Fayoumi S, Ligueros-Saylan M, Sarangapani R, et al. Pharmacokinetics and pharmacodynamics of LCZ696, a novel dual-acting angiotensin receptor-neprilysin inhibitor (ARNi). J Clin Pharmacol. 2010;50(4):401–14.
Mills J, Vardeny O. The role of neprilysin inhibitors in cardiovascular disease. Curr Heart Fail Rep. 2015;12(6):389–94.
King JB, Bress AP, Reese AD, Munger MA. Neprilysin inhibition in heart failure with reduced ejection fraction: a clinical review. Pharmacotherapy. 2015;35(9):823–37.
Sun C, Wang W, Bao X, Chen D, Mei S, Ma J, et al. Quantification of Rhodojaponin II and Rhodojaponin III in rat plasma by ultra-performance liquid chromatography-tandem mass spectrometry. Int J Anal Chem. 2024;2024:6386570.
Kommu S, Berg RL. The efficacy and safety of Sacubitril/Valsartan compared to Valsartan in patients with heart failure and mildly reduced and preserved ejection fractions: a systematic review and meta-analysis of randomized controlled trials. J Clin Med. 2024;13(6):1572.
Pravalika K, Subhashini V. Analytical review on newly approved antidiabetic and antihypertensive drugs. Int J Drug Deliv Technol. 2024;14(1):537–44.
Chakraborty A, Jayaseelan K, Rathinam S, KS K, KN K. Bioanalytical methods and extraction techniques for the quantification of hydrochlorothiazide and its pharmaceutical combinations: a comprehensive review. Acta Chromatogr. 2024. https://doi.org/10.1556/1326.2023.01187.
Wang S, Wang Y, Deng Y, Zhang J, Jiang X, Yu J, et al. Sacubitril/valsartan: research progress of multi-channel therapy for cardiorenal syndrome. Front Pharmacol. 2023;14:1167260. https://doi.org/10.3389/fphar.2023.1167260.
Raja R, Kumari S, Khan MU, Ayaz A, Jaffar D, Mohamad Z, et al. Antihypertensive effects of Sacubitril/Valsartan versus Olmesartan: an updated systemic review and meta-analysis of randomized controlled trials. Cureus. 2023;15(11):e48692. https://doi.org/10.7759/cureus.48692.
Patel MA, Pandya P, Mehta M, Kothari S. Method development and validation of some antihypertensive drugs by RP-HPLC: a comparative study. Eur Chem Bull. 2023;12(10):4668–79.
Gurav L, et al. A robust RP-HPLC analytical method development and validation of Cilnidipine and Olmesartan in antihypertensive formulations. RRJ Pharm Nano. 2023;11:001.
Lamprecht DG, Saseen JJ, Shaw PB. Clinical conundrums involving statin drug-drug interactions. Prog Cardiovasc Dis. 2022;75:83–9. https://doi.org/10.1016/j.pcad.2022.11.002.
Kido K, Colvin BM, Szymanski TW, Guglin M. Sacubitril/Valsartan off-label uses for heart failure. J Card Fail. 2022;28(7):1185–201. https://doi.org/10.1016/j.cardfail.2022.03.348.
Avataneo V, Fanelli E, De Nicolò A, Rabbia F, Palermiti A, Pappaccogli M, et al. A non-invasive method for detection of antihypertensive drugs in biological fluids: the salivary therapeutic drug monitoring. Front Pharmacol. 2022;12:755184. https://doi.org/10.3389/fphar.2021.755184.
González R, Torrado G, Arribas JM, Peña MA. Development of an analytical method for the determination and quantification of N-Nitrosodimethylamine in Olmesartan by HPLC-MS/MS. Microchem J. 2022;179:107402. https://doi.org/10.1016/j.microc.2022.107402.
Zhang R, Sun X, Li Y, He W, Zhu H, Liu B, et al. The efficacy and safety of Sacubitril/Valsartan in heart failure patients: a review. J Cardiovasc Pharmacol Ther. 2022;27:10742484211058681. https://doi.org/10.1177/10742484211058681.
Patel P, Dave H. Analytical method development and validation of tertiary combinations of antihypertensive drugs: a review. Int J Pharm Sci Res. 2022;13(9):3447–57. https://doi.org/10.13040/IJPSR.0975-8232.13(9).3447-57.
Jaglinska K, Polak B, Klimek-Turek A, Fornal E, Stachniuk A, Trzpil A, et al. Comparison of the determination of some antihypertensive drugs in clinical human plasma samples by solvent front position extraction and precipitation modes. Molecules. 2023;28:2213. https://doi.org/10.3390/molecules28052213.
El-Didamoony MA, Elsadek ME, Baraka MM, Ibrahim SM, Sebaiy MM. Analytical methods for determination of certain antihypertensive drugs. Biomed J Sci Tech Res. 2021;34(2). BJSTR.MS.ID.005513.
Wagmann L, Vollmer AC, Lauder L, Mahfoud F, Meyer MR. Assessing adherence to antihypertensive medication by means of dose-dependent reference plasma concentration ranges and ultra-high performance liquid chromatography-ion trap mass spectrometry analysis. Molecules. 2021;26:1495. https://doi.org/10.3390/molecules26051495.
Jaglińska K, Polak B, Klimek-Turek A, Błaszczyk R, Wysokiński A, Dzido TH. Preparation of antihypertensive drugs in biological matrix with solvent front position extraction for LC-MS/MS analysis. Molecules. 2022;27(1):205. https://doi.org/10.3390/molecules27010205.
Lai PM, Xue JH, Xie MJ, Ye JH, Tian KJ, Ling JY, et al. Emerging trends in Sacubitril/Valsartan research: a bibliometric analysis of the years 1995–2021. Medicine. 2022;101(31):e29398. https://doi.org/10.1097/MD.0000000000029398.
Reddy R, Reddy I, Jagannath D, Nagesh M, Manne R. Bio-analytical method development and validation of Olmesartan in human EDTA plasma using LC-MS/MS detection method. J Appl Pharm Sci. 2020;4:97–150.
Richter LHJ, Jacobs CM, Mahfoud F, Kindermann I, Böhm M, Meyer MR. Development and application of a LC-HRMS/MS method for analyzing antihypertensive drugs in oral fluid for monitoring drug adherence. Anal Chim Acta. 2019;1070:69–79. https://doi.org/10.1016/j.aca.2019.04.026.
Haque SKM, Alsawalha M. Analytical methods for the quantitation of amlodipine besylate and atorvastatin calcium in pharmaceutical dosage form and biological fluids. Int J Appl Pharm. 2019;11(3):5–15. https://doi.org/10.22159/ijap.2019v11i3.32566.
Kumar A, Dwivedi SP, Prasad T. Method validation for simultaneous quantification of Olmesartan and Hydrochlorothiazide in human plasma using LC-MS/MS and its application through bioequivalence study in healthy volunteers. Front Pharmacol. 2019;10:810. https://doi.org/10.3389/fphar.2019.00810.
Jhund PS, McMurray JJV. The neprilysin pathway in heart failure: a review and guide on the use of Sacubitril/Valsartan. Heart. 2016;102(17):1342–7. https://doi.org/10.1136/heartjnl-2014-306775.
Bharti T, Mishra R, Rajput C, Singhal R. Analytical method development and validation of assay for Olmesartan Medoxomil in formulated product by reverse phase ultra performance liquid chromatography. J Pharm Anal. 2016;3:215–22.
Sunitha N, Marihal SC, Sravanthi J, Venu A, Rao BN, Rao BA. Method development and validation of RP-HPLC method for the simultaneous estimation of Olmesartan and Cilnidipine in bulk and formulations. Int J Pharm Res Allied Sci. 2015;4(3):127–35.
Beg S, Sharma G, Katare OP, Lohan S, Singh B. Development and validation of a stability-indicating liquid chromatographic method for estimating Olmesartan Medoxomil using quality by design. J Chromatogr Sci. 2015;53(7):1048–59. https://doi.org/10.1093/chromsci/bmu165.
Raja B, Lakshmana Rao A. Development and validation of a reversed phase HPLC method for simultaneous estimation of Olmesartan and Hydrochlorothiazide in combined tablet dosage form. Int J Res Pharm Chem. 2011;1(3)..
Downloads
Published
How to Cite
Issue
Section
License
This work is licensed under a Creative Commons Attribution 4.0 International License.
You are free to:
- Share — copy and redistribute the material in any medium or format
- Adapt — remix, transform, and build upon the material for any purpose, even commercially.
Terms:
- Attribution — You must give appropriate credit, provide a link to the license, and indicate if changes were made. You may do so in any reasonable manner, but not in any way that suggests the licensor endorses you or your use.
- No additional restrictions — You may not apply legal terms or technological measures that legally restrict others from doing anything the license permits.
