顶空毛细管气相色谱法测定盐酸克伦特罗中溶剂残留

Determination of Residual Organic Solvents in Clenbuterol Hydrochloride by Headspace Gas Chromatography

目的:建立盐酸克伦特罗中乙醇、异丙醇、二氯甲烷3种有机溶剂残留量的分析测定方法。方法:顶空毛细管气相色谱法,FID检测器,进样口温度为140℃,检测器温度为250℃,DB-624石英毛细管柱(30 m×0.32 mm,1.8μm),起始柱温为40℃,维持7 min,再以30℃·min^(-1)升至200℃,维持5 min。顶空瓶平衡温度为80℃,平衡时间为45 min。结果:被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度和回收率良好。结论:本方法灵敏、准确、可靠,可用于盐酸克伦特罗溶剂残留的质量控制。

Objective：To establish a headspace GC method for the determination of residual solvents in clenbuterol hydrochloride. Method：Ethanol,isopropanol and dichloromethane were separated on a DB-624 capillary column（30 m×0.32 mm,1.8μm） in a headspace sampling mode.The carrying gas was nitrogen.The inlet and FID detector temperature was 140℃and 250℃,respectively. The column temperature was maintained at 40℃for 7 min,then was raised to 200℃at the rate of 30℃·min-1 and maintained at 200℃for 5 min.The equilibrium temperature and time was 80℃.and 45 min,respectively.Result：The measured solvents were separated completely.The calibration curve of each solvent showed a good linear relationship with promising precision and accuracy.Conclusion： The established method is simple and reliable,which can be used in the determination of residual solvents in clenbuterol hydrochloride.