DEVELOPMENT AND VALIDATION OF SENSITIVE LC-ESI-MS/MS METHOD FOR THE SIMULTANEOUS ESTIMATION OF DAPAGLIFLOZIN AND SAXAGLIPTIN IN HUMAN PLASMA

  • Phanindra Adluri Research Scholar, Mewar University, Chittorgarh, Rajasthan, India
  • Shravan Kumar Y Research Supervisor, Mewar University, Chittorgarh, Rajasthan, India

Abstract

Objective: To develop and validate a sensitive liquid chromatography-electrospray ionization-tandem mass spectrometric (LC-ESI-MS/MS) technique for the quantification of dapagliflozin and saxagliptin in plasma by linagliptin as internal standard.


Methods: Chromatography was achieved on hypersil C18 (50 mmx4 mm) 5 µ analytical column with 0.1% formic acid and acetonitrile (25:75 V/V) as mobile phase at 0.7 ml/min flow rate. Dapagliflozin, saxagliptin, and linagliptin were detected at m/z 409.14/135.0, m/z 316.2/180.13 and m/z 472.54/456.21 respectively. Drugs and internal standard were extracted by LLE (liquid-liquid extraction).


Results: Developed technique was validated over 0.5-1500.0 ng/ml linear concentration range for dapagliflozin and 2.00-2000.0 ng/ml for saxagliptin. This method established with intra-batch and inter-batch precision within 2.44-8.12% and 1.25-7.14 % for dapagliflozin and 1.84-7.5 % and 1.02–6.00 % for saxagliptin. This method established with intra-batch and inter-batch accuracy for dapagliflozin within 98.86-103% and 96.98-102 % respectively and for saxagliptin within 98.05-109.06 % and 97.00-104.00 % respectively.


Conclusion: Both dapagliflozin and saxagliptin were stable during three freeze-thaw cycles, long term and bench-top stability studies. The developed method was useful for the routine analysis of dapagliflozin and saxagliptin simultaneously in plasma samples.

Keywords: Dapagliflozin, Saxagliptin, LC-ESI-MS/MS, Validation, Precision and Accuracy

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How to Cite
Adluri, P., and S. K. Y. “DEVELOPMENT AND VALIDATION OF SENSITIVE LC-ESI-MS/MS METHOD FOR THE SIMULTANEOUS ESTIMATION OF DAPAGLIFLOZIN AND SAXAGLIPTIN IN HUMAN PLASMA”. International Journal of Pharmacy and Pharmaceutical Sciences, Vol. 11, no. 4, Feb. 2019, pp. 55-59, doi:10.22159/ijpps.2019v11i4.31249.
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