DEVELOPMENT AND VALIDATION OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF DAPAGLIFLOZIN AND ITS IMPURITIES IN TABLET DOSAGE FORM
Keywords:Dapagliflozin, High-performance liquid chromatography method, Impurity
Objective: The aim of the present work is the development of new, sensitive, specific, and accurate high-performance liquid chromatographic method for the separation and determination of dapagliflozin and its impurities in tablet dosage form.
Methods: The chromatographic separation of drug and its impurities was achieved using Hypersil BDS C18 column (250 mm × 4.6 mm, 5 μ) with mobile phase consisted of mobile phase-A (Buffer pH 6.5) and mobile phase-B (acetonitrile:water 90:10) by gradient program at a flow rate of 1 mL/min with ultraviolet detection at 245 nm.
Results: Dapagliflozin and its impurities A, B, C, D, E, and impurity-F were successfully eluted at the retention time of 16.95, 2.72, 7.82, 10.58, 21.11, 30.37, and 34.36 min, respectively, with good resolution. The method was validated according to the international conference on harmonization guidelines. The validation results showed good precision, accuracy, linearity, specificity, sensitivity, and robustness.
Conclusion: Successful separation and determination of dapagliflozin and its six impurities were achieved by the proposed method. The developed method can be applied for the routine analysis of dapagliflozin and its impurities in pharmaceutical formulations.
Committee for Medicinal Products for Human Use, European Medicine Agency. Forxiga-Assessment Report. Available from: http://www.ema.europa.eu/docs/en_GB/document_library/EPAR_-Public_assessment_report/human/002322/WC500136024.pdf. [Last cited on 2016 Nov 16].
Therapeutic Goods Administration, Department of Health and Ageing, Australian Government. Australian Public Assessment Report for Dapagliflozin Propanediol Monohydrate. Available from: https://www.tga.gov.au/sites/default/files/auspar-dapagliflozin-propanediol-monohydrate-130114.pdf. [Last cited on 2016 Nov 16].
Drug Bank. Dapagliflozin. Available from: https://www.drugbank.ca/drugs/DB06292. [Last cited on 2016 Nov 14].
Federal Register International Conferences on Harmonization. Draft Revised Guidance on Impurities in New Drug Substances, Q3A(R); 2000. p. 45085-90.
Veeprho Pharmaceuticals. Dapagliflozin Impurity. Available from: https://www.veeprhopharma.com/dapagliflozin-impurity-manufacturer-supplier.php. [Last cited on 2016 Nov 14].
Mante GV, Gupta KR, Hemke AT. Estimation of dapagliflozin from its tablet formulation by UV spectrometry. Pharm Methods 2017;8:102-7.
Sanagapati M, Dhanalakshmi K, Nagarjunareddy G, Kavitha. B. Method development and validation of dapagliflozin API by UV spectroscopy. Int J Pharm Sci Rev Res 2014;27:270-2.
Jani BR, Shah KV, Kapupara PP. Development and validation of UV spectroscopic first derivative method for simultaneous estimation of dapagliflozin and metformin hydrochloride in synthetic mixture. J Bioequiv Stud 2015;1:1-8.
Chitra KP, Eswaraiah MC, Rao MV. Unique UV spectrophotometric method for reckoning of dapagliflozin in bulk and pharmaceutical dosage forms. J Chem Pharm Res 2015;7:45-9.
Jeyabaskaran M, Rambabu C, Dhanalakshmi B. RP-HPLC method development and validation of dapagliflozin in bulk and tablet formulation. Int J Pharm Anal Res 2013;2:221-6.
Sanagapati M, Dhanalakshmi K, Nagarjunareddy G, Sreenivasa S. Development and validation of a RP-HPLC method for the estimation of dapagliflozin in API. Int J Pharm Sci Res 2014;5:5394-7.
Yunoos M, Sankar DG. A validated stability indicating high performance liquid chromatographic method for simultaneous determination of metformin HCL and dapagliflozin in bulk drug and tablet dosage form. Asian J Pharm Clin Res 2015;8:320-6.
Shyamala, Nidhi B, Kavitha M, Pooja, Sharma JV. Validated RP-HPLC method for simultaneous estimation of metformin hydrochloride and dapagliflozin in tablet dosage form. Am J Biol Pharm Res 2015;2:109-3.
Debata J, Kumar S, Jha SK, Khan A. A new RP-HPLC method development and validation of dapagliflozin in bulk and tablet dosage form. Int J Drug Dev Res 2017;9:48-51.
Patel KJ, Chaudhary AB, Bhadani SM, Raval RJ. Stability indicating RP-HPLC method development and validation for estimation of dapagliflozin and metformin HCl. World J Pharm Pharm Sci 2017;6:796-809.
Verma MV, Patel CJ, Patel MM. Development and stability indicating HPLC method for dapagliflozin in API and pharmaceutical dosage form. Int J Appl Pharm 2017;9:1618-32.
Prameela KL, Veni PR, Narayana PV, Haribabu B. Development and validation of stability indicating high performance liquid chromatography method with photodiode array detection for the simultaneous estimation hypoglycemic agents, dapagliflozin and metformin. Int J Pharm Bio Sci 2017;8:328-36.
Patel A, Maheshwari D. Development and validation of UV spectrophotometric method and RP-HPLC method for simultaneous estimation of dapagliflozin propanediol and glimepiride in synthetic mixture. Eur J Pharm Med Res 2017;4:416-34.
Phani RS, Prasad KR, Mallu UR. A study of new method development, validation and forced degradation for simultaneous analysis of dapagliflozin and saxagliptin in pharmaceutical dosage form by HPLC method. Pharm Chem 2017;9:96-103.
Aubry AF, Gu H, Magnier R, Morgan L, Xu X, Tirmenstein M, et al. Validated LC-MS/MS methods for the determination of dapagliflozin, a sodium-glucose co-transporter 2 inhibitor in normal and ZDF rat plasma. Bioanalysis 2010;2:2001-9.
International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use. Validation of Analytical Procedures: Text and Methodology ICH Q2 (R1); 2005.
Daksh S, Goyal A, Pandiya CK. Validation of analytical methods-strategies and significance. Int J Res Dev Pharm Life Sci 2015;4:1489 97.
Tsvetkova B, Pencheva I, Zlatkov A, Peikov P. High performance liquid chromatographic assay of indomethacin and its related substances in tablet dosage forms. Int J Pharm Pharm Sci 2012;4:549-52.
Oruganti SS. Development and validation of analytical methods for the determination of impurities in some selected drug substances using high performance liquid chromatographic technique. Int Curr Pharm Res 2016;8:49-53.
Ravichandran V, Shalini S, Sundram KM, Rajak H. Validation of analytical methods-strategies and importance. Int J Pharm Pharm Sci 2010;2:18-22.
How to Cite
The publication is licensed under CC By and is open access. Copyright is with author and allowed to retain publishing rights without restrictions.