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

This study presents the development and validation of a rapid and reproducible hydrophilic interaction liquid chromatography (HILIC) method for the simultaneous quantification of remogliflozin etabonate (RE), vildagliptin (VD), and metformin (MF) in a pharmaceutical formulation. The research employed a face-centered central composite experimental design to optimize chromatographic conditions, ensuring a robust and efficient analytical procedure. The optimized method utilized a HILIC column with an isocratic mobile phase consisting of acetonitrile (65% v/v) and 20 mM phosphate buffer (35% v/v, pH 6), achieving separation of the three analytes within 3.6 minutes at a flow rate of 1.4 mL/min. Detection was performed at 210 nm. The method was thoroughly validated according to ICH guidelines, demonstrating excellent linearity across concentration ranges of 20–150 µg/mL for RE, 10–75 µg/mL for VD, and 50–750 µg/mL for MF, with regression coefficients (r2) greater than 0.999. Precision and accuracy were confirmed by low percentage relative deviation and relative error, and high percentage recovery of added standard drugs. Robustness was established through a half-normal probability plot and Pareto chart, indicating minimal influence from slight variations in single factors. This validated HILIC method provides an accurate and reproducible tool for routine quality control of pharmaceutical preparations containing this triple combination of antidiabetic drugs.

This study presents the development and validation of a rapid and reproducible hydrophilic interaction liquid chromatography (HILIC) method for the simultaneous quantification of remogliflozin etabonate (RE), vildagliptin (VD), and metformin (MF) in a pharmaceutical formulation. The research employed a face-centered central composite experimental design to optimize chromatographic conditions, ensuring a robust and efficient analytical procedure. The optimized method utilized a HILIC column with an isocratic mobile phase consisting of acetonitrile (65% v/v) and 20 mM phosphate buffer (35% v/v, pH 6), achieving separation of the three analytes within 3.6 minutes at a flow rate of 1.4 mL/min. Detection was performed at 210 nm. The method was thoroughly validated according to ICH guidelines, demonstrating excellent linearity across concentration ranges of 20–150 µg/mL for RE, 10–75 µg/mL for VD, and 50–750 µg/mL for MF, with regression coefficients (r2) greater than 0.999. Precision and accuracy were confirmed by low percentage relative deviation and relative error, and high percentage recovery of added standard drugs. Robustness was established through a half-normal probability plot and Pareto chart, indicating minimal influence from slight variations in single factors. This validated HILIC method provides an accurate and reproducible tool for routine quality control of pharmaceutical preparations containing this triple combination of antidiabetic drugs. Research Background and Significance The increasing prevalence of diabetes mellitus has necessitated the development of effective pharmaceutical formulations combining multiple antidiabetic agents to improve therapeutic efficacy and patient compliance. Remogliflozin etabonate (RE), vildagliptin (VD), and metformin (MF) rep