Abstract

A NEW ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE QUANTITATIVE DETERMINATION OF SITAGLIPTIN AND SIMVASTATIN IN BULK FORM AND COMBINED MARKETED PHARMACEUTICAL DOSAGE FORM BY USING REVERSE PHASE-HPLC

Sandhya Goulikar*

Abstract

A new, simple, precise, accurate and reproducible RP-HPLC method for Simultaneous estimation of Sitagliptin and Simvastatin in bulk and pharmaceutical formulations. Separation of Sitagliptin and Simvastatin was successfully achieved on a Phenomenex Luna C18 (4.6×250mm, 5μm) particle size or equivalent in an isocratic mode utilizing Acetonitrile: Phosphate Buffer (pH-4.6) (45:55 v/v) at a flow rate of 1.0mL/min and elutes was monitored at 245nm, with a retention time of 2.102 and 3.537 minutes for Sitagliptin and Simvastatin respectively. The method was validated and the response was found to be linear in the drug concentration range of 6μg/mL to 14μg/mL for Sitagliptin and 18μg/mL to 42μg/mL for Simvastatin. The values of the slope and the correlation coefficient were found to be 77824 and 0.999 for Sitagliptin and 10515 and 0.999 for Simvastatin respectively. The LOD and LOQ for Sitagliptin were found to be 0.6μg/mL and 1.8μg/mL respectively. The LOD and LOQ for Simvastatin were found to be 0.8 μg/mL and 2.4μg/mL respectively. This method was found to be good percentage recovery for Sitagliptin and Simvastatin were found to be 100.351 and 100.93 respectively indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample so, the method specifically determines the analytes in the sample without interference from excipients of tablet dosage forms. The method was extensively validated according to ICH guidelines for Linearity, Range, Accuracy, Precision, Specificity and Robustness.

Keywords: Sitagliptin and Simvastatin, RP-HPLC, Accuracy, Precision, ICH Guidelines.