QUALITY BY DESIGN APPROACH FOR THE DEVELOPMENT AND VALIDATION OF SAXAGLIPTIN BY RP-HPLC WITH APPLICATION TO FORMULATED FORMS

Quality by Design (QbD) is a philosophy that refines the level of knowledge associated with a product that uses process understanding to deliver a product with the desired critical quality attributes. The objective of this present study was to develop and demonstrate an integrated multivariate approach to develop and quantify the constituent concentrations of saxagliptin drug in its pure and formulated forms. The method was developed using a mobile phase acetonitrile: water (pH3), (20:80 v/v) on an Agilent, TC C18 (250 × 4.6 mm) 5μm column and flow rate 1.0 ml/min which was optimized with help of design expert software and validated according to ICH Q2 guideline and application of this method to different stress condition of saxagliptin. The detector linearity was established in concentrations ranging from 10-90μgmL-1, the regression coefficient was 0.9993. The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.003 and 0.010?gmL-1, respectively. The percentage relative standard deviations for robustness and ruggedness were observed within the range of 0.28 and 0.57. The drug was subjected to acidic, alkali, neutral, oxidative, heat and photo degradation stress. Drug shows significantly degraded in acidic and alkali condition while remain stable in other conditions. The high recovery and low relative standard deviation confirm the suitability of these methods can be employed for the routine analysis of tablet containing saxagliptin