Abstract

DEVELOPMENT AND VALIDATION OF RELATED SUBSTANCES METHOD BY HPLC FOR ANALYSIS OF TRELAGLIPTIN SUCCINATE

Dr. Ajit Anerao*, Vikas Mundekar, Satish John and Dr. Nitin Pradhan

ABSTRACT

A simple, selective, precise reversed phase high-pressure liquid chromatography (HPLC) method has been developed and validated for estimation of related substances of Trelagliptin succinate active pharmaceutical ingredient (API). Efficient chromatographic separation was achieved on a Cosmosil 5μm particles size, 250mm × 4.6mm column and detection was performed at 225 nm wavelength. Linear regression analysis data for the calibration plot showed there was a good linear relationship between response and concentration of API and related impurities. The method was validated for accuracy, precision, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines. Statistical analysis proved the method was precise, reproducible, selective, specific, and accurate for analysis of Trelagliptin succinate and its related impurities. HIGHLIGHTS  Related substances method is developed for quantification of specified and unspecified impurities of Trelagliptin succinate.  Reliability and reproducibility of results is confirmed by performing analytical method validation as per ICH guideline.  Force degradation study is carried out by exposing the API to stress conditions and found all degradants are separating from the main component and can be quantified accurately.  Response factor, LOD and LOQ of specified impurities are reported.

Keywords: Trelagliptin succinate, method development and validation, HPLC.