Development and Validation of High-Performance Liquid Chromatographic Method for Determination of Dapagliflozin and Its Impurities in Tablet Dosage Form

Abstract

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.

Qualitative and Quantitative Determination of Dapagliflozin Propanediol Monohydrate and Its Related Substances and Degradation Products Using LC-MS and Preparative Chromatography Methods

“…The retention time of DPG was longer 22.965 minutes in the proposed method compared to the reported method. However, the proposed method in our study was found more sensitive (LOD of 8.59 ng/mL) with shorter runtime of 70 minutes than the reported one 14 . The proposed method also offers an advantage in determining the relationship between the impurity profile and the stability profile.…”

“…The published HPLC-VIS method for the determination of DPG and its six impurities used different chromatographic conditions (mobile phase and detection wavelength) 14 . The retention time of DPG was 16.95 min, with a LOD of 0.065 µg/mL, a linearity range was 0.20-13.00 µg/mL, and a total runtime of 75 minutes.…”

“…Drug related substances may also produce from the degradation of active pharmaceutical ingredient API or formulated drug product [6][7][8][9] . The determination of dapagliflozin alone or in combination with other drugs was performed using (UV) spectrometry [10][11] , thin layer chromatography TLC [11][12][13] , reverse phase highperformance liquid chromatography (RP-HPLC) 11,[14][15][16][17] and LC-mass spectrometry 11,[18][19][20] . However, one HPLC method was reported for the determination of DPG with six impurities in tablets dosage form.…”

“…However, one HPLC method was reported for the determination of DPG with six impurities in tablets dosage form. 'The chromatographic separation of dapagliflozin and its six impurities was performed using Hypersil BDS C18 column (length of 250 mm, 4.6 mm i.d and 5 μm particle size) with the eluent consisted of buffer pH 6.5 (A) and acetonitrile: water 90:10 (B) by gradient elution mode at a flow rate of 1 mL/min with UV detection at 245 nm 14 .…”

Stability Indicating HPLC Method Development and Validation for Simultaneous Estimation of Dapagliflozin and Metformin Tablet Dosage Form

“…DAPA is a SGLT-2 inhibitor indicated for managing diabetes mellitus Type 2. When combined with diet and exercise in adults, DAPA helps to improve glycemic control by inhibiting glucose resorption in the proximal tubule of the nephron and causing glycosuria [1][2][3][4][5][6][7][8].…”