IMPLEMENTATION OF ANALYTICAL QBD IN STABILITY-INDICATING RP-UPLC METHOD DEVELOPMENT AND VALIDATION FOR COMBINED QUANTIFICATION OF VILDAGLIPTIN AND PIOGLITAZONE

Abstract

Concurrent detection of Vildagliptin and Pioglitazone in pharmaceutical formulations is the primary goal of this work, which aims to establish an RP-UPLC technique. An improved chromatographic environment was the goal of the methodology's Central Composite Design (CCD) phase. Three independent variables—temperature, mobile phase composition, and flow rate—were included in the design that was implemented using Design-Expert® software. With a UV detector set to 212 nm, the column temperature was maintained at 30°C, and a flow rate of 0.31 mL/min, the RP-UPLC analysis was carried out. For Pioglitazone and Vildagliptin, the approach was validated by analysing linearity, precision (%RSD), recovery rates, and forced degradation trials. In the advanced RP-UPLC method, Vildagliptin (12.5-75 µg/mL) and Pioglitazone (3.75-22.5 µg/mL) demonstrated strong linearity. Vildagliptin had a Limits of Detection of 0.44 µg/mL and pioglitazone had a quantification threshold of 1.32 µg/mL, while pioglitazone had a threshold of 4.02 µg/mL. For both Vildagliptin and Pioglitazone, the recovery rates ranged from 99.08% to 100.98%, and the methodology's Relative Standard Deviation (RSD) was less than 2% in terms of accuracy. Both chemicals were susceptible to oxidative and photolytic reactions, according to studies on synthetic deterioration. Using the validated RP-UPLC method, which was designed in accordance with Quality by Design (QbD) principles, the pharmaceutical formulations including Vildagliptin and Pioglitazone were simultaneously quantified. Cases of induced degradation proved the stability, sensitivity, and extraordinary linearity of the approach.