“Development And Validation Of An Rp-Hplc Method For Estimating Process-Related Impurities In Antidiabetic Drugs”

Abstract

There has been ever increasing interest in impurities present in Active Pharmaceutical Ingredient’s (API’s). Nowadays, not only purity profile but also impurity profile has become mandatory according to the various regulatory authorities. The study aimed to develop and validate a reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of process-related impurities in Dapagliflozin, Vildagliptin, and Sitagliptin. The method was optimized using various mobile phases and validated according to ICH guidelines for parameters including linearity, accuracy, precision, robustness, LOD, and LOQ. The optimized method employed an Agilent Poroshell C18 column (150 mm × 4.6 mm, 5 µm), with a mobile phase of acetonitrile and 0.05% orthophosphoric acid in water (30:70, v/v), at a flow rate of 1.0 mL/min, and detection at 210 nm. The method exhibited good linearity (r² > 0.998), accuracy (recovery within 98–102%), and precision (RSD < 2%). The method is suitable for routine quality control of impurities in antidiabetic formulations.

Regulatory bodies across the globe have established compre­hensive guidelines to ensure that impurity profiling is rigorously conducted during the development and manufacturing of pharma­ceuticals. These guidelines are designed to protect public health by setting acceptable limits for impurities and mandating robust ana­lytical methods for their detection and quantification. Thus impurity profiling is a cornerstone of pharmaceutical development, ensuring that drug products are safe, effective, and of high quality. Regulatory guidelines such as FDA (Food and Drug Administration, USA), EMA (European Medicines Agency), Pharmacopoeias etc. The presence of impurities can accelerate the degradation of drug products, thereby reducing their shelf life and stability. Stability stud­ies are conducted to understand how impurities develop over time and under various storage conditions, which is essential for establish­ing appropriate storage guidelines and expiration dates.