COST EFFECTIVE ACCURATE & PRECISE ANALYTICAL METHOD VALIDATION FOR THE CONTENT ESTIMATION OF N-NITROSODIMETHYLAMINE & N-NITROSODIETHYLAMINE IN OLMESARTAN MEDOXOMIL BY GCMS

摘要

A simple, precise and accurate GCMS method was validated for estimation the content estimation of NNitrosodimethylamine (NDMA) & N-Nitrosodiethylamine (NDEA) in olmesartan medoxomil (OLM) in drug substances.The content was determined by GCMS on DB-CAM 30.0 m Χ 0.32 mm, 0.5μm Capillary column and helium was used ascarrier gas, using methanol as diluent at column flow rate of 2.0 mL/min and Ion source temperature & Interfacetemperature at 200oC and Detector gain mode relative to tuning file with acquisition mode Q3 SIM. The method wasvalidated as per ICH guidelines for Specificity, linearity, LOQ accuracy and LOQ precision. The method shows goodlinearity over the concentration range of 0.24-3.61 for NDMA and 0.07-0.99 for NDEA Concentration in ppm (μg/g)(r2=0.998) for olmesartan. The average percentage recoveries were in the range of 108.0-113.4% and 97.6-106.7% forN-Nitrosodimethylamine (NDMA) & N-Nitrosodiethylamine (NDEA) in olmesartan medoxomil, respectively. The limits ofdetection (LODs) were 0.23 concentrations in ppm (μg/g) and 0.10 concentrations in ppm (μg/g) for NDMA and NDEA,and limits of quantification (LOQs) were 0.71 μg/g and 0.31μg/g, respectively. Therefore, the proposed method can beapplied for routine analysis of the bulk drugs as well as combined pharmaceutical dosage forms of olmesartanmedoxomil.