Sivagami B, Sharmil Kumar. L.M, Chandrasekar. R, Niranjan Babu. M
Sivagami B1*, Sharmil Kumar. L.M, Chandrasekar. R2, Niranjan Babu. M3
1Associate Professor, Department of Pharmaceutical Analysis, Seven Hills College of Pharmacy, Tirupati, 517561, Chitoor (Dist) Andhrapradesh.
2Associate Professor, Department of Pharmacognosy, Seven Hills College of Pharmacy, Tirupati, 517561, Chitoor (Dist) Andhrapradesh.
3Professor, Department of Pharmacognosy, Seven Hills College of Pharmacy, Tirupati, 517561, Chitoor (Dist) Andhrapradesh.
Volume - 15,
Issue - 11,
Year - 2022
Background: A simple new novel, accurate, robust and precise RP-HPLC method was developed and validated for the simultaneous quantification of Rilpivirine and Dolutegravir in bulk and marketed tablet formulations. Methods: The method development was carried out by using INERTSIL ODS column (250×4.6mm, 5µm), by isocratic approach using a mixture of Phosphate Buffer (pH 6.8): Acetonitrile in the ratio of (35: 65) as mobile phase. The flow rate was 1.0 ml/min, 259 nm as detection wavelength. Results: The retention time of 3.285 min was observed for Dolutegravir and 4.635 min for Rilpivirine. Dolutegravir percentage purity was 99.97% and 100.63% for Rilpivirine. The system suitability parameters such as theoretical plate and tailing factor for Dolutegravir and Rilpivirine was observed in the range of 3209, 1.13 and 5210, 1.11and was found to be within the limit. The linear was observed in the concentration ranges of 50µg – 250µg for Dolutegravir and 30µg - 150µg for Rilpivirine and correlation coefficient (r2) value for Dolutegravir was 0.999 and 0.999 for Rilpivirine. The percentage RSD for repeatability was observed to be within the acceptance limit 0.1 and 0.7. The percentage RSD for intermediate precision was 0.4 and 0.8. The precision study was precise, robust, and repeatable. The LOD values were 3 and 3.02 and LOQ values were 9.98 and 10.01. Conclusion: Hence the optimized RP-HPLC method can be used for simultaneous quantification and concurrent analysis of Dolutegravir and Rilpivirine in API and combined dosage formulations.
Cite this article:
Sivagami B, Sharmil Kumar. L.M, Chandrasekar. R, Niranjan Babu. M. Development and Validation for the Simultaneous Estimation of Rilpivirine and Dolutegravir in Bulk and Pharmaceutical Dosage Forms by RP-HPLC Method. Research Journal of Pharmacy and Technology. 2022; 15(11):5302-6. doi: 10.52711/0974-360X.2022.00893
Sivagami B, Sharmil Kumar. L.M, Chandrasekar. R, Niranjan Babu. M. Development and Validation for the Simultaneous Estimation of Rilpivirine and Dolutegravir in Bulk and Pharmaceutical Dosage Forms by RP-HPLC Method. Research Journal of Pharmacy and Technology. 2022; 15(11):5302-6. doi: 10.52711/0974-360X.2022.00893 Available on: https://rjptonline.org/AbstractView.aspx?PID=2022-15-11-78
1. Min S, Song I, Borland J, Chen S, Lou Y, Fujiwara T, Piscitelli SC: Pharmacokinetics and safety of S/GSK1349572, a next-generation HIV integrase inhibitor, in healthy volunteers. Antimicrob Agents Chemother. 2010; 54(1):254-8.
2. Dow DE, Bartlett JA: Dolutegravir, the Second-Generation of Integrase Strand Transfer Inhibitors (INSTIs) for the Treatment of HIV. Infect Dis Ther. 2014; 3(2):83-102.
3. Hare S, Smith SJ, Metifiot M, Jaxa-Chamiec A, Pommier Y, Hughes SH, Cherepanov P: Structural and functional analyses of the second-generation integrase strand transfer inhibitor dolutegravir (S/GSK1349572). Mol Pharmacol. 2011; 80(4):565-72.
4. Putcharoen O, Kerr SJ, Ruxrungtham K: An update on clinical utility of rilpivirine in the management of HIV infection in treatment-naive patients. HIV AIDS (Auckl). 2013, 16; 5:231-41.
5. Usach I, Melis V, Peris JE: Non-nucleoside reverse transcriptase inhibitors: a review on pharmacokinetics, pharmacodynamics, safety and tolerability. J Int AIDS Soc. 2013, 4; 16:1-14.
6. Ford N, Lee J, Andrieux-Meyer I, Calmy A: Safety, efficacy, and pharmacokinetics of rilpivirine: systematic review with an emphasis on resource-limited settings. HIV AIDS (Auckl). 2011; 3:35-44.
7. Cozzi V, Charbe N, Baldelli S, et al. Development and Validation of a Chromatographic Ultraviolet Method for the Simultaneous Quantification of Dolutegravir and Rilpivirine in Human Plasma. Ther Drug Monit. 2016; 38(3):407-413.
8. Tempestilli M, Ammassari A, D'Avolio A, et al. Development and validation of an HPLC-UV method for quantification of elvitegravir and two other new antiretrovirals, dolutegravir and rilpivirine, in the plasma of HIV-positive patients. Biomed Chromatogr. 2018; e4274.
9. Venkatesan S, Kannappan N, Mannemala SS. Stability-Indicating HPLC Method for the Simultaneous Determination of HIV Tablet Containing Emtricitabine, Tenofovir Disoproxil Fumarate, and Rilpivirine Hydrochloride in Pharmaceutical Dosage Forms. Int Sch Res Notices. 2014; 2014:849149.
10. Gorja Ashok, Sumanta Mondal Development and Validation of Stability Indicating Method for the Simultaneous Estimation of Batcaver Sulfate, Lamivudine and Dolutegravir Sodium in Pharmaceutical Dosage forms by RP-HPLC Saudi J. Med. Pharm. Sci., 2018, 4(2): 289-296
11. Sapna M Rathod, Paresh U Patel. Development and Validation of RP – HPLC Method for Estimation of Lamivudine and Dolutegravir Sodium in Synthetic Mixture. Research J. Pharm. and Tech 2020; 13(6): 2864-2868.
12. Yusuff Ismail , M.Vijaya Vara Prasad , S. M. Shaheedha , Mohammad Habeeb A New Stability Indicating RP-HPLC Method Development and Validation for the Simultaneous Estimation of Dolutegravir and Rilpivirine in Bulk and its Dosage Forms. Iranian Journal of Pharmaceutical Sciences 2019: 15 (4): 53-72.
13. Venkatnarayana M, Siva Jyothi N Development of Validation and Stability Indicating Method of Anti-HIV Dolutegravir Drug and its Related Impurities by Using RP-HPLC. J Chromatogr Sep Tech. 2020, 11:426.
14. Saravanan. R, Somanathan. T, Gavaskar D, Tamilvanan M. Analytical Method Development and Validation of Stability Indicating assay method of analysis for Dolutegravir/Lamivudine/Tenofovir Disoproxil Fumarate tablets using High Performance Liquid Chromatography Research Journal of Pharmacy and Technology. 2021; 14(5):2434-9.
15. Bhavar GB, Pekamwar SS, Aher KB, Thorat RS, Chaudhari SR. High-Performance Liquid Chromatographic and High-Performance Thin-Layer Chromatographic Method for the Quantitative Estimation of Dolutegravir Sodium in Bulk Drug and Pharmaceutical Dosage Form. Sci Pharm. 2016; 84(2):305-320.
16. Grégoire M, Deslandes G, Renaud C, et al. A liquid chromatography-tandem mass spectrometry assay for quantification of rilpivirine and dolutegravir in human plasma. J Chromatogr B Analyt Technol Biomed Life Sci. 2014; 971:1-9.
17. Prathipati PK, Mandal S, Destache CJ. Simultaneous quantification of tenofovir, emtricitabine, rilpivirine, elvitegravir and dolutegravir in mouse biological matrices by LC-MS/MS and its application to a pharmacokinetic study. J Pharm Biomed Anal. 2016; 129:473-481.
18. Simiele M, Ariaudo A, De Nicolò A, et al. UPLC-MS/MS method for the simultaneous quantification of three new antiretroviral drugs, dolutegravir, elvitegravir and rilpivirine, and other thirteen antiretroviral agents plus cobicistat and ritonavir boosters in human plasma. J Pharm Biomed Anal. 2017; 138:223-230.
19. Khaleel N and Abdul Rahaman SK Stability-Indicating RP-UPLC Method for the Simultaneous Determination of Dolutegravir and Rilpivirine in Bulk and Pharmaceutical Dosage Form Der Pharmacia Lettre, 2019, 11 (2): 29-39.
20. Saravanan. R, Somanathan. T, Gavaskar D, Tamilvanan M. Analytical Method Development and Validation of Stability Indicating assay method of analysis for Dolutegravir/Lamivudine/Tenofovir Disoproxil Fumarate tablets using High Performance Liquid Chromatography Research Journal of Pharmacy and Technology. 2021; 14(5):2434-9.