Determination of Residual Organic Solvents in Erlotinib Hydrochloride by Headspace Gas Chromatography / 中国药师

ABSTRACT

Objective:To establish a headspace capillary gas chromatography method for the determination of residual solvents in erlotinib hydrochloride .Methods:A DB-624 capillary column (30 m ×0.53 mm, 3.0 μm) was used and the carrier gas was nitro-gen.The flow rate was 2.0 ml· min-1 and the inlet temperature was 190℃.The FID detector temperature was 230 ℃.The column temperature program was with the initial temperature of 35℃( maitaining 8 min) , risen to 170℃with the rate of 28℃· min-1 ( main-taining 8 min) , and then risen to 200℃with the rate of 32℃· min-1 ( maintaining 7 min) .The headspace vial temperature was 100℃and the time was 30 min.Results:Ethanol, isopropanol, methylene chloride and n-butanol had a good linear relationship within the range of 0.68-409.14 μg· ml-1 (r=0.999 8),0.67-404.88 μg· ml-1 (r=0.999 8),1.71-51.31μg· ml-1 (r=0.999 7) and 0.72-431.12 μg· ml-1(r=0.999 8), respectively.The average recovery was 99.0% (RSD=0.41%, n=9), 100.2%(RSD=0.52%, n=9),97.1%(RSD=1.75%, n =9) and 102.5% (RSD=1.08%, n=9), respectively.Conclusion: The method is simple and accurate , which can be used for the determination of four residual organic solvents in erlotinib hydrochloride .