Stability Indicating RP-HPLC Method Development and Validation for Simultaneous Estimation of Dapagliflozin Propanediol Monohydrate and Teneligliptin Hydrobromide Hydrate in Synthetic Mixture

For the quantitative measurement of Dapagliflozin propanediol monohydrate and Teneligliptin hydrobromide hydrate in synthetic mixture form in the presence of its degradants, precise, accurate, robust, cost-effective, and isocratic stability indicating RP-HPLC method was developed and validated. The mobile phase comprises [Methanol: 20 mM Ammonium formate (70:30 v/v)] at a flow rate of 1.0 ml/min, injection volume of 20 µl, and UV detection at 225 nm. Separation was accomplished using Gemini, C18 column. Teneligliptin hydrobromide hydrate and Dapagliflozin propanediol monohydrate were eluted with retention times of 6.65 minutes and 4.20 minutes, respectively. This procedure was approved following ICH guideline Q2 (R1). The calibration plots for Dapagliflozin propanediol monohydrate and Teneligliptin hydrobromide hydrate have correlation coefficients of 0.9995 and 0.9996 over the concentration ranges of 5-100 µg/ml and 10-200 µg/ml respectively. For Dapagliflozin propanediol monohydrate and Teneligliptin hydrobromide hydrate, accuracy ranged from 99.81-100.78% and 99.13-100.69%, respectively. For Dapagliflozin propanediol monohydrate and Teneligliptin hydrobromide hydrate, the LOD was found to be 0.947 µg/ml and 1.355 µg/ml. In contrast, the LOQ was 2.869 µg/ml and 4.107 µg/ml, respectively. The findings demonstrated the applicability of the devised approach for routine analysis of Teneligliptin hydrobromide hydrate and Dapagliflozin propanediol monohydrate in a synthetic mixture form with its degradants.

Keywords:

Dapagliflozin propanediol monohydrate, Teneligliptin hydrobromide hydrate, RP- HPLC Stability indicating method, Validation,

PDF

___

1. "Drug Profile and Information of Dapagliflozin Propanediol Monohydrate", October 2023, Available from:
2. "Drug Profile and Information of Dapagliflozin Propanediol Monohydrate", October 2023, Available from:
3. Vyas AJ, Gol DA, Patel AI, Patel AB, Patel NK, Chavda JR, Lumbhani A, Chudasama A. Implementing Analytical Quality by Design (AQbD) Approach for Simultaneous Estimation of Tadalafil and Macitentan by RP-HPLC Method. Analytical Chemistry Letters. 2021;11(4):539-552. Available from:
4. Vyas AJ, Patel SM, Patel AB, Patel AI, Patel NK. Stability testing: An Essential study for Vaccine Formulation Development. Asian Journal of Pharmaceutical Analysis. 2022;12(1):29-6. Available from:
5. Vyas AJ, Visana NM, Patel AI, Patel AB, Patel NK. Analytical Quality by Design in Stress Testing or Stability-Indicating Method. Asian Journal of Pharmaceutical Analysis. 2021;11(2):170-178. Available from:
6. Patel AI, Prajapati KB, Jolapara SH, Vyas AJ, Patel AB, Patel NK, Pandey MN. RP-HPLC method for determination of gemfibrozil using central composite design (CCD). Research Journal of Pharmacy and Technology. 2021;14(6):3009-3014. Available from:
7. Vyas AJ, Jha SA, Patel AB, Patel AI, Shah SR. Review on simultaneous equation method (Vierodt's method). Asian Journal of Pharmaceutical Analysis. 2022;12(2):149-156. Available from:
8. Patel AI, Ram K, Guttikar S, Vyas AJ, Patel AB, Patel NK, Trivedi V. Rapid, sensitive and simple LC-MS/MS method development and validation for estimation of phenytoin in human plasma by using deuterated internal standard. Research Journal of Pharmacy and Technology. 2021;14(6):2937-2944. Available from:
9. Vaghela A, Patel AB, Patel AI, Vyas AJ, Patel NK. Sample Preparation in Bioanalysis: A Review. International Journal of Scientific & Technology Research. 2016;5(5):6-10. Available from:
10. Patel AB, Asnani AH, Vyas AJ, Patel NK, Patel AI. A brief review on genotoxic impurities in pharmaceuticals. Asian Journal of Pharmaceutical Research. 2021;11(3):187-193. Available from:
11. Patel AB, Bundheliya AR, Vyas AJ, Patel NK, Patel AI. A Review on Metal Impurities in Pharmaceutical. Asian Journal of Pharmaceutical Analysis. 2021;11(3):212-222. Available from:
12. Vyas AJ, Godhaniya JP, Patel AI, Patel AB, Patel NK, Chudasama A, Shah SR. A review on carcinogenic impurities found in marketed drugs and strategies for its determination by analytical methods. Asian Journal of Pharmaceutical Analysis. 2021;11(2):159-169. Available from:
13. Patel AI, Prajapati KB, Vyas AJ, Patel AB, Patel NK. Determination and validation of phthalate impurities in milk by UV-spectrophotometry method. Pharma Science Monitor. 2021;10(4):49-58.
14. Vyas AJ, Rajput M, Patel NK, Chotaliya U, Patel AB, Patel AI. Determination of genotoxic Impurity by Chromatographic Method. An International Journal of Pharmaceutical Sciences. 2017;8(2):24-31. Available from:
15. Vyas AJ, Taviyad M, Patel NK, Chotaliya U, Singh S, Patel AB, Patel AI. Chromatographic Method Development and Validation for Related Substance. Pharma Science Monitor. 2017;8(2):32-39.
16. Vyas AJ, Rathod N, Patel AI, Prajapati R, Patel NK, Patel AB. Analytical Method Development and Validation of Stability Indicating Method and Related Substance by Using RP-HPLC of Drug Substance. Pharma Science Monitor. 2017;8(2):409-419.
17. Bakshi M, Singh S. Development of validated stability-indicating assay methods-critical review. Journal of Pharm. and Bio. Ana. 2002;28:1011-40. Available from:
18. Vyas AJ, Gol DA, Patel AI, Patel AB, Patel NK, Chudasama A. A stress degradation kinetic study of Tadalafil bulk and tablet dosage form by UV Spectrophotometry. Asian Journal of Pharmaceutical Analysis. 2020;10(4):177-181. Available from:
19. Patel A, Jadeja P, Mashru R. Analytical Method Development and Validation for Simultaneous Estimation of Dapagliflozin and Teneligliptin Hydrobromide Hydrate from Synthetic Mixture by Three Different UV Spectrophotometric Methods. World Journal of Pharmaceutical Research. 2022;11(7):770-783. Available from:
20. Debata J, Kumar S, Jha SK, Khan A. A New RP-HPLC Method Development and Validation of Dapagliflozin in Bulk and Tablet Dosage Form. International Journal of Drug Development and Research. 2017;9(2):48-51. Available from:
21. Sravanthi S, Zarin N, Shruthi B, Ramya KD, Manjeera A. A New Analytical Method Development and Validation for the Estimation of Dapagliflozin by Using Reverse Phase-High Performance Liquid Chromatography International Journal of Advanced Research in Medical & Pharmaceutical Sciences. 2021;6(4):13-20. Available from:
22. Manasa S, Dhanalakshmi K, Reddy GN, Sreenivasa S. Method development and validation of dapagliflozin in API by RP-HPLC and UV-spectroscopy. International Journal of Pharmaceutical Sciences and Drug Research. 2014;6(3):250-252. Available from:
23. Basha SS, Sravanthi P. Development and Validation of Dapagliflozin by Reversed-Phase High-Performance Liquid Chromatography Method and It's Forced Degradation Studies. Asian Journal of Pharmaceutical Clinical Research. 2017;10(11):101-105. Available from: 24. Vaghela YV, Patani P, Patel D. Development and Validation of Stability Indicating Estimation Method of Dapagliflozin in Its Tablet Dosage Form. International Journal of Research and Analytical Reviews. 2019;6(2):206-213.
25. Bodiwala KB, Shah J, Sureja DK, Dhameliya TM. Generation of predictive models for oxidative degradation kinetics of dapagliflozin with the applications of DOE and stability indicating HPLC method, International Journal of Chemical Kinetics. 2022;54(12):712-725. Available from:
26. Nagwanshi S, Aher S, Bachhav R. Stability Indicating RP-HPLC Method Development and Validation of Dapagliflozin in Bulk and Tablet Dosage Form. World Journal of Pharmacy and Pharmaceutical Sciences. 2021;10(9):2251-2262.
27. Sanagapati M, Dhanalakshmi K, Reddy NG, Kavitha B. Method Development and Validation of Dapagliflozin API by UV Spectroscopy. International Journal of Pharmaceutical Sciences Review and Research. 2014;27(1):270-272. Available from:
28. Biswas B, Kumar M, Sharma JB, Saini V, Bhatt S. Method Development and Validation for Estimation of Teneligliptin in Tablet Dosage Form by RP-HPLC. Research Journal of Pharmacy and Technology. 2020;13(4):1774-1778. Available from:
29. Reddy GS, Swetha V, Venu G, Pavani J. Analytical Method Development and Validation of Teneligliptin Hydrobromide Hydrate in Active Pharmaceutical Ingredient by using RP-HPLC. International Journal of Biology, Pharmacy and Allied Sciences. 2021;10(7):2250-2262. Available from:
30. Lokhande P. Analytical Method Development and Validation of Teneligliptin by using RP-HPLC with ICH Guidelines. International Journal of Trend in Scientific Research and Development. 2019;3(3):259-263. Available from:
31. Luhar SV, Pandya KR, Jani GK, Narkhed SB. Simultaneous Estimation of Teneligliptin Hydrobromide Hydrate and its Degradation Product by RP-HPLC Method. Journal of Pharmaceutical Science and Bioscientific Research. 2016;6(3):254-261. Available from:
32. Yadav N, Goyal A. Method development and validation of Teneligliptin in pharmaceutical dosage form by UV spectrophotometric methods. International Journal of Pharmaceutical Chemistry and Analysis. 2017;4(3):54-58. Available from:
33. Ghuge BS, Pendhari SS, Malode PA, Anantwar SP. Development and Validation of Simple UV Spectrophotometric Method for The Determination of Teneligliptin Hydrobromide Hydrate in API and its Bulk Dosage Form. International Journal for Pharmaceutical Research Scholars. 2017;6(2):44-53. Available from:
34. Gadi VL, Devanaboyina N. Method Development and Validation for Simultaneous Estimation of Dapagliflozin & Saxagliptin by RP-HPLC Method. World Journal of Pharmaceutical and Medical Research. 2020;6(7):243-248.
35. Urooj A, Shyam Sundar P, Vasanthi R, Raja MA, Dutt KR, Rao KNV. Development and Validation of RP-HPLC Method for Simultaneous Estimation of Dapagliflozin and Metformin in Bulk and in Synthetic Mixture. World Journal of Pharmacy and Pharmaceutical Sciences. 2017; 6(7):2139-2150. Available from:
36. Gupta A, Mishra SK. A Novel Analytical Method for Simultaneous Quantification of Dapagliflozin and Sitagliptin by Reverse Phase High Performance Liquid Chromatography. Journal of Medical Pharmaceutical and Allied Sciences. 2021;10(3):2861-2865. Available from:
37. Rao SS, Srinivas S, Gupta VR, Babu VJ. Stability Indicating Method Development and Validation of Dapagliflozin and Saxagliptin Drugs by Using RP-HPLC Method. Journal of Global Trends in Pharmaceutical Sciences. 2021;12(3):9554-9559.
38. Ahmad S, Usman R, Shaikh T, Imran MD, Akhtar R. Development and Validation of UV Spectrophotometric Method for Estimation of Saxagliptin and Dapagliflozin in Bulk and Dosage Form. International Journal of Pharmaceutical Sciences and Research. 2021;12(4): 2185-2192. Available from:
39. Janil S, Shukla R, Patel P, Mehta B, Detholia K. Quantitative estimation of sitagliptin and dapagliflozin propanediol monohydrate in synthetic mixture using 1st order derrivative spectroscopy simultaneous spectrophotometric analysis. International Journal of Pharmaceutical Chemistry and Analysis. 2022;9(1):28-34. Available from:
40. Shirisha K, Amina begum K, Sravya K, Swarna K, Neelima K, Rao SS. Analytical Method Development and Validation of Teneligliptin and Metformin HCL by using RP-HPLC Method. Journal of Global Trends in Pharmaceutical Sciences. 2020;11(3):8051-8056.
41. Patel F, Dalwadi P, Patel D, Mehta N. Development and Validation of RP-HPLC Method for Simultaneous Estimation of Teneligliptin Hydrobromide Hydrate and Rosuvastatin Calcium in Synthetic Mixture. International Journal of All Research Education and Scientific Methods. 2021;9(4), 2712-2719. Available from:
42. Vashi D, Gamit D. Development and Validation of RP-HPLC Method for Simultaneous Estimation of Remogliflozin Etabonate and Teneligliptin in Pharmaceutical Dosage Form. World Journal of Pharmacy and Pharmaceutical Sciences. 2022;11(8):1504-1516. Available from:
43. Gheewala JA, Maheshwari DG. Development and Validation of UV Spectrophotometric Method and RP-HPLC Method for Simultaneous Estimation of Teneligliptin and Pioglitazone in Synthetic Mixture. Asian Journal of Pharmaceutical Technology & Innovation. 2017;23(5):66-78.
44. Chotaliya UJ, Dobariya HJ, Barad DL, Vyas AJ, Gol DA. Stability Indicating RP-HPLC-DAD Method For Simultaneous Estimation of Atorvastatin Calcium and Teneligliptin Hydrobromide Hydrate in Synthetic Mixture. Analytical Chemistry Letters. 2022;12(5):629-638. Available from:
45. Mane SS, Mhaske MS. Development and Stability Indicating RP-HPLC Method for Simultaneous Estimation of Metformin HCL and Teneligliptin HBR Hydrate in Bulk and Pharmaceutical Dosage Form. Indo American Journal of Pharmaceutical Science. 2022;9(6):499-518. Available from:
46. Solanki MS, Goyal PK. Simultaneous Estimation of Teneligliptin and Metformin Hydrochloride in Tablet Formulation by UV Spectrophotometric Method. Chemistry Research Journal. 2021;6(6):160-165. Available from:
47. Vashi D, Gamit D. Development and Validation of UV- Spectroscopic Method for Simultaneous Estimation of Remogliflozin Etabonate and Teneligliptin in Bulk and Pharmaceutical Dosage Form by Simultaneous Equation Method. World Journal of Pharmaceutical and Life Science. 2022;8(8):149-153.
48. ICH-Harmonized Tripartite Guideline (2005) Validation of analytical procedures: text and methodology Q2 (R1). In: International conference on harmonization, IFPMA, Geneva, Switzerland.