Research Journal of Pharmacy and Technology

Open Access Open Access  Restricted Access Subscription Access
Open Access Open Access Open Access  Restricted Access Restricted Access Subscription Access

Stability Indicating Hplc Method Development and Validation For Simultaneous Estimation of Metformin and Empagliflozin in Bulk And Pharmaceutical Dosage Form


Affiliations
1 School of Pharmacy, Swami Ramanand Teerth Marathwada University, Vishnupuri, Nanded 431606, (M.S.), India
2 D. K. Patil Institute of Pharmacy, Loha 431708, Dist-Nanded, (M.S.), India
     

   Subscribe/Renew Journal


In the present work, simple, accurate and rapid stability indicating RP-HPLC method has been developed for the simultaneous estimation of Metformin and Empagliflozin in bulk and tablet dosage form. Separation of analytes was carried out on Ascentis C18 HPLC column (4.6 x 150 mm, 5 μm) using a mobile phase of 0.1% orthophosphoric acid and acetonitrile (60:40, v/v), at a flow rate of 1.0mL/min and measurement carried out at UV 260 nm. The validation parameters namely linearity, sensitivity, selectivity, specificity. robustness, precision and accuracy were determined. The peak area response-concentration curve was linear, over the concentration range of 125-750 μg/mL for Metformin and 1.25-7.50 μg/mL for Empagliflozin with quantitation limits of 4.59 μg/mL for Metformin, and 0.08 μg/mL for Empagliflozin. The proposed method was successfully validated for the determination of Metformin and Empagliflozin simultaneously in combined tablet dosage form. The performance of the present method was compared with available RP-HPLC methods and found to be rapid and economical. The proposed stability-indicating RP-HPLC method can be successfully applied to quality control and drug analysis.

Keywords

Metformin, Empagliflozin, RP-HPLC, ICH Guidelines, Stability-indicating method.
Subscription Login to verify subscription
User
Notifications
Font Size


  • Olokoba AB, et al. Type 2 Diabetes Mellitus: A Review of Current Trends. Oman Medical Journal. 2012; 27(4): 269-273.

  • Seuring T, et al. The economic costs of type 2 diabetes: A Global Systematic Review. Pharmacoeconomics. 2015; 33(8): 811-831.

  • Zheng Y, et al. Global aetiology and epidemiology of type 2 diabetes mellitus and its complications. Nature Reviews Endocrinology. 2018; 14(2): 88-98.

  • Ripsin CM, et al. Management of blood glucose in type 2 diabetes mellitus. American Family Physician. 2009; 79(1): 29-36.

  • Hu FB, et al. Diet, lifestyle, and the risk of type 2 diabetes mellitus in women. The New England Journal of Medicine. 2001; 345(11): 790-797.

  • Grarup N, et al. Genetic susceptibility to type 2 diabetes and obesity: from genome-wide association studies to rare variants and beyond. Diabetologia. 2014; 57: 1528-1541.

  • American Diabetes Association. 8. Pharmacologic approaches to glycemic treatment: standards of medical care in diabetes-2018. Diabetes Care. 2018; 41(1): S73-S85.

  • Rojas C, et al. Link J, Meinicke T, Macha S. Pharmacokinetics of fixed-dose combinations of empagliflozin/metformin compared with individual tablets in healthy subjects. International Journal of Clinical Pharmacology and Therapeutics. 2016; 54(4): 282-292.

  • Bays H. From victim to ally: the kidney as an emerging target for the treatment of diabetes mellitus. Current Medical Research and Opinion. 2009; 25(3): 671-681.

  • Rena G, et al. The mechanisms of action of metformin. Diabetologia. 2017; 60(9): 1577-1585.

  • Patil SD, et al. Development and validation of UV spectrophotometric method for Simultaneous estimation of Empagliflozin and Metformin hydrochloride in bulk drugs. Asian Journal of Pharmaceutical Analysis. 2017; 7(2): 117-123.

  • Ayoub BM. Development and validation of simple spectrophotometric and chemometric methods for simultaneous determination of Empagliflozin and metformin: Applied to the recently approved pharmaceutical formulation, Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy. 2016; 168: 118-122.

  • Patil SD, et al. Development and Validation of Simple UVSpectrophotometric Method for the Determination of Empagliflozin. Asian Journal of Pharmaceutical Analysis. 2017; 7(1): 18-22.

  • Shinde GS, et al. Quantitative Estimation and Validation of Metformin Hydrochloride and Gliclazide in their Tablet Dosage Form by RP-HPLC. Research Journal of Science and Technology. 2019; 11(3): 201-207.

  • Baokar SB, et al. Development and Validation of RP-HPLC Method for Simultaneous Estimation of Vildagliptin and Metformin. Research Journal of Pharmaceutical Dosage Forms and Technology. 2013; 5(2): 95-98.

  • Pulla RP, et al. Simultaneous Estimation of Metformin HCL and Sitagliptin Phosphate in Tablet Dosage Forms by RP-HPLC. Research Journal of Pharmacy and Technology. 2011; 4(4): 646- 649.

  • Siridevi MP, et al. RP-HPLC Method for Quantification of Empagliflozin in Pharmaceutical Formulation. Asian Journal of Pharmacy and Technology. 2019; 9(3): 208-211. 18. Patil SD, et al. Development and Validation of Stability Indicating RP-HPLC Method for Empagliflozin. Asian Journal of Pharmaceutical Analysis. 2016; 6(4): 201-206.

  • Ayoub BM, Mowaka S. LC-MS/MS Determination of Empagliflozin and Metformin. Journal of Chromatographic Science. 2017; 55(7): 742-747.

  • Gopal NM, Sridhar C. A validated stability-indicating ultraperformance liquid chromatographic method for simultaneous determination of metformin hydrochloride and empagliflozin in bulk drug and tablet dosage form. International Journal of Applied Pharmaceutics. 2017; 9 (3): 45-50.

  • Riaz MK, et al. Simultaneous Determination, Validation and Forced Degradation Studies of Metformin and Empagliflozin Using New HPLC Analytical Method. Latin American Journal of Pharmacy. 2020; 39(11): 2257-2265

  • Swarupa GP, et al. Development and validation of stabilityindicating reversed-phase high-pressure liquid chromatography method for simultaneous estimation of metformin and empagliflozin in bulk and tablet dosage form. Asian Journal of Pharmaceutical and Clinical Research. 2016; 9(1): 126-135.

  • Godasu SK, Sreenivas SA. A new validated RP-HPLC method for the determination of metformin HCL and empagliflozin in its bulk and pharmaceutical dosage forms. International Journal of 1. Pharmaceutical Sciences and Research. 2017; 8(5): 2223-2232.

  • Pathan M, Kshirsagar A. Development of Validated Stability Indicating Method by Rp-HPLC for Simultaneous Estimation of Meropenem and Vaborbactam in Bulk and Pharmaceutical Formulation. International Journal of Pharmacy and Pharmaceutical Sciences. 2019; 11(7): 102-108.

  • Kokkirala TK, Suryakala D. Stability indicating RP-HPLC Method Development and Validation for the Estimation of Sofosbuvir, Velpatasvir and Voxilaprevir in Bulk and Pharmaceutical dosage form. Research Journal of Pharmacy and Technology. 2020; 13(11): 5063-5071.

  • Bhavya B, et al. Stability Indicating RP-HPLC Method Development and Validation for Simultaneous Estimation of Albendazole and Ivermectin in Pharmaceutical Dosage form. Asian Journal of Pharmaceutical Analysis. 2017; 7(1): 6-14.

  • Phalguna Y, et al. Analytical Method Development and Validation for the Estimation of Sacubitril and Valsartan in Combined Pharmaceutical Dosage Forms by RP-HPLC. Asian Journal of Research in Pharmaceutical Sciences. 2018; 8(1): 09-16.

  • ICH, The European Agency for the Evaluation of Medicinal Products. ICH Topic Q2B Note for Guideline on Validation of Analytical Procedures: Methodology. GPMP/ICH/281/95, 1996.

  • ICH Guidance on Analytical Method Validation, International Convention on Quality for the Pharmaceutical Industry: Toronto, Canada, 2002.

  • ICH, Technical Requirements for the Registration of Pharmaceutical for Human Use; Validation of Analytical Procedures: Text and Methodology Q2 (R1); IFPMA: Geneva, Switzerland, 2005.

  • ICH, Q1A (R2) Stability Testing of New Drug Substances and Products. International Conference on Harmonization, Geneva, 2003.

  • ICH, Q1B, Stability Testing: Photostability Testing of New Drug Substances and Products, International Conference on Harmonization. IFPMA: Geneva, Switzerland, 1996.


Abstract Views: 89

PDF Views: 0




  • Stability Indicating Hplc Method Development and Validation For Simultaneous Estimation of Metformin and Empagliflozin in Bulk And Pharmaceutical Dosage Form

Abstract Views: 89  |  PDF Views: 0

Authors

Mudassar Ahemadkhan Pathan
School of Pharmacy, Swami Ramanand Teerth Marathwada University, Vishnupuri, Nanded 431606, (M.S.), India
Ajay Kshirsagar
D. K. Patil Institute of Pharmacy, Loha 431708, Dist-Nanded, (M.S.), India

Abstract


In the present work, simple, accurate and rapid stability indicating RP-HPLC method has been developed for the simultaneous estimation of Metformin and Empagliflozin in bulk and tablet dosage form. Separation of analytes was carried out on Ascentis C18 HPLC column (4.6 x 150 mm, 5 μm) using a mobile phase of 0.1% orthophosphoric acid and acetonitrile (60:40, v/v), at a flow rate of 1.0mL/min and measurement carried out at UV 260 nm. The validation parameters namely linearity, sensitivity, selectivity, specificity. robustness, precision and accuracy were determined. The peak area response-concentration curve was linear, over the concentration range of 125-750 μg/mL for Metformin and 1.25-7.50 μg/mL for Empagliflozin with quantitation limits of 4.59 μg/mL for Metformin, and 0.08 μg/mL for Empagliflozin. The proposed method was successfully validated for the determination of Metformin and Empagliflozin simultaneously in combined tablet dosage form. The performance of the present method was compared with available RP-HPLC methods and found to be rapid and economical. The proposed stability-indicating RP-HPLC method can be successfully applied to quality control and drug analysis.

Keywords


Metformin, Empagliflozin, RP-HPLC, ICH Guidelines, Stability-indicating method.

References