Multivariate optimization of liquid chromatographic conditions for determination of dapagliflozin and saxagliptin, application to an in vitro dissolution and stability studies

Abstract

Background Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of dapagliflozin and saxagliptin in pharmaceutical dosage form. Response surface methodology was employed for optimization of experimental conditions using three factors such as organic phase (%), pH of aqueous phase, and flow rate of mobile phase. Results Virtuous separation of analytes was achieved with mobile phase consisted of acetonitrile: phosphate buffer, pH 5.8 (26:74% v/v) with flow rate 0.96 mL/min using SPOLAR C18 column (250 × 4.6 mm, 5 μ) with run time 6 min and UV detection at 236 nm. Retention time for dapagliflozin and saxagliptin were found to be 3.5 and 5.0 min, respectively. Method was validated as per ICH guidelines. The plot between peak area vs concentration for dapagliflozin and saxagliptin were rectilinear in the range of 0.2-300 μg/mL and 0.1-150 μg/mL respectively with detection and quantification limits were 0.061 and 0.18 μg/mL for dapagliflozin and 0.014 and 0.043 μg/mL for saxagliptin, respectively. Conclusion The proposed method was exploited for assay, in vitro dissolution, and stability studies of target drugs in marketed dosage form.

New Eco-friendly UV-spectroscopic Methods for Simultaneous Assessment of Dapagliflozin, Saxagliptin and Metformin in Ternary Mixture

“…3,4 Qternmet XR ® consisting of dapagliflozin (10 mg), saxagliptin (5 mg), and metformin hydrochloride (1000 mg) formulated as tablets (extended release) is a fixed-dose combination that improves the blood sugar level in individuals with diabetes mellitus (Type 2) if given in conjunction with controlled regime of diet and regular workout. 9-11 Literature survey disclosed numerous analytical approaches for the assessment of DPZ, SGT and MTH independently and in combined dosage form by means of UV-spectrophotometry, 12-16 HPLC [3][4][17][18][19][20][21] and HPTLC. 22,23 Moreover, few approaches were described for the assessment of DPZ, SGT and MTH in mixed formulation/synthetic mixture using HPLC 10 and HPTLC.…”

An Experimental Design Approach to Quantitative Expression for Quality Control of a Multicomponent Antidiabetic Formulation by the HILIC Method

“…This is because an experimental design is based on predefined objectives and the identification of variable factors having a significant interactive effect on the analysis. The importance of experimental design is increased due to the incorporation of quality by design as a regulatory requirement of analytical method development used for the quality control of pharmaceutical formulations targeting the safety of patients, as part of pharmaceutical product development [ 47 , 48 , 49 ]. The literature features the use of surface response methodologies, such as central composite design for the development of the HILIC method [ 50 , 51 ].…”