Cost Effective Accurate and Precise Analytical Method Development of Content Estimation of N-Nitrosodimethyl Amine and N-Nitrosodiethyl Amine in Olmesartan Medoxomil by GC-MS

Abstract

A simple, precise and accurate GCMS method was developed for estimation the content estimation of N-Nitrosodimethylamine (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 as carrier gas, using methanol as diluent at column flow rate of 2.0 mL/min and Ion source temperature & Interface temperature at 200ºC and Detector gain mode relative to tuning file with acquisition mode Q3 SIM. The method was developed and evaluated for validation parameter as per ICH guidelines for Specificity, linearity, accuracy and precision. The method shows good linearity over the range of 10%-150% for NDMA and NDEA for olmesartan. The average percentage recoveries were found within predefined acceptance criteria (10% and 100%) for N-Nitrosodimethylamine (NDMA) & N-Nitrosodiethylamine (NDEA) in olmesartan medoxomil, respectively. Therefore, the proposed method can be applied for routine analysis of the bulk drugs as well as combined pharmaceutical dosage forms of olmesartan medoxomil. Keywords: Olmesartan medoxomil (OLM), N-Nitrosodimethylamine (NDMA) &, N-Nitrosodiethylamine (NDEA) GCMS, Validation, Analytical validation.