Development and validation of reversed phase HPLC method for the determination of vildagliptin using an experimental design

Abstract

A simple, robust and fast reversed phase HPLC method was developed and validated with UV detection (210 nm) for routine determination of vildagliptin. Chromatographic analysis was performed with mobile phase containing a mixture of 10 mM phosphate buffer (pH 4.6) and acetonitrile (85: 15, v/v) with flow rate of 1.0 mL/min. The procedure was validated as per International Conference on Harmonization (ICH) guidelines for linearity (correlation coefficient r 2 = 0.999), accuracy, intermediate precision and robustness. Experimental design was used during validation to calculate method robustness and intermediate precision. For testing robustness three factors were considered: pH of buffer, flow rate and percentage (v/v) of acetonitrile. From the analysis it was observed that an increase in the flow rate results in a decrease of drug found concentration, while the pH of buffer and percentage of organic modifier have no significant effect on the response. To measure intermediate precision, the variables considered were: analyst, equipment and number of days. The relative standard deviation (RSD) value (2.25%, n = 24) indicated a good precision for analytical method. The proposed method was simple, accurate, precise, sensitive and cost effective for further determination of vildagliptin.