Residual Solvents by GC-HS Procedure for Etoricoxib: Method Development and Validation Report

Abstract

The intent of this research paper was to describe a “headspace gas chromatography (HGC)” procedure development and its completely validation for the analysis of residuals of methanol (MTL), isopropyl alcohol (IPL), t-butanol (TBL), toluene (TLE) and dimethylformamide (DFL) simultaneously in Etoricoxib (EIB). The experimentations are done on HGC system fitting with flame ionization type detector employing DB-624 silica fused capillary column (stationary phase) and nitrogen gas (mobile phase). The injector port and detector port temperatures were kept at 200 oC and 260 oC, respectively. N-methyl pyrrolidone was diluent. The MTL, IPL, TBL, TLE, and DFL detection (LOD) and quantitation (LOQ) values were much smaller than their ICH specification level concentrations. The linear corelation evaluated through range of LOQ to 150% of ICH specification level concentrations for MTL, IPL, TBL, TLE, and DFL of ICH. The regression coefficients for MTL, IPL, TBL, TLE, and DFL were ≥0.9950, and the diagrams of theoretic residuals concentration versus gotten peak response are linear. The HGC procedure proposed was represented by great accuracy, precision, ruggedness and specificity. For a minimum of 48 hr, the EIB sample with MTL, IPL, TBL, TLE and DFL is stable while managed to keep at ambient temperature. The current developed and completely validated HGC procedure can run effectively for EIB residual solvents (MTL, IPL, TBL, TLE and DFL) assessing in active pharma ingredient production.