Stability Indicating Method Development and Validation of Vildagliptin and Dapagliflozin in Bulk and in Marketed Formulation by UHPLC Method

Aim

Vildagliptin and Dapagliflozin in fixed-dose combination is used for treatment of Type II Diabetes Mellitus. The key objective of the current research work is to develop a new stability-indicating UHPLC method for the simultaneous estimation of Vildagliptin and Dapagliflozin in tablet dosage form as no such method is available.

Materials and Methods

A successful separation was achieved by using Agilent column C₁₈ (4.6×100 mm) and mobile phase of Methanol: 0.1% Orthophosphoric acid (78:22) at a flow rate of 1.0 mL and detection wavelength of 234 nm. The forced degradation study was performed at extreme forced conditions such as hydrolysis with acid and base, peroxide oxidation and photolytic degradation, following ICH guidelines.

Results

The retention time for Vildagliptin and Dapagliflozin was 2.3 and 4.7 min respectively. The suggested approach yields linear responses for Vildagliptin and Dapagliflozin in the concentration of the 50-250 μg/mL and 5-25 μg/mL, respectively. Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 1.04 μg/mL and 3.15 μg/mL for Vildagliptin and 0.24 μg/mL and 0.73 μg/mL for Dapagliflozin, respectively. In the exposed conditions, the drugs did not exhibit any significant degradation.

Conclusion

The UHPLC approach that was recommended proved to be highly sensitive, accurate, precise, robust and stability indicating. The method can be successfully adopted for the routine analysis for the simultaneous estimation of the Vildagliptin and Dapagliflozin in bulk and pharmaceutical dosage form.