【摘要】 目的:建立顶空气相色谱法测定安立生坦原料中甲醇、乙醇、叔丁基甲基醚、乙酸乙酯、二氧六环、N,N-二甲基甲酰胺等残留量的方法。方法:采用HP-5（30 m×0.53 mm,1.5μm）石英毛细管柱,载气为高纯氮气,FID检测器,采用程序升温和顶空进样,柱温35℃保持5 min,再以20℃·min^-1升温至110℃,保持5 min。结果:6种残留溶剂的分离度符合要求,线性关系良好（r≥0.999 0）。回收率均在99.3%¹05.2%范围内,3批安立生坦样品检测结果均符合限度要求。结论:该方法检测灵敏、准确,可用于检测安立生坦原料药的残留溶剂。更多还原

【Abstract】 Objective: To establish a headspace GC method for the determination of the residual solvents（ methanol,ethanol,methyl-butyl ether,ethyl acetate,dioxane and N,N-dimethylformamide） in ambrisentan. Methods: An HP-5 capillary column（ 30 m× 0. 53 mm,1. 5 μm） was used with nitrogen as the carrier gas and an FID as the detector. The temperature program and headspace injection mode were used. The initial column temperature was kept at 35℃ for 5min,and then was raised to 110℃ at the rate of 20℃ ·min^-1. Results: The 6 solvents were well separated,and a good linearity was obtained within the designed range for each solvent with the correlation coefficients no less than 0. 999 0. The average recoveries were from 99. 3% to 105. 2%. All the residual solvents in ambrisentan were within the limited quantity range. Conclusion: The method is highly sensitive and accurate,which can be applied in the determination of the residual solvents of ambrisentan.更多还原