顶空气相色谱法测定淫羊藿提取物中的残留有机溶剂  

ASE-GC determination of residual solvents in extracts of Herba Epimedii

作　　者：邓桂凤[1] 戴伟东[1] 姚彤炜[1] 

机构地区：[1]浙江大学药学院药物分析与药物代谢研究所,杭州310058

出　　处：《药物分析杂志》2008年第11期1955-1960,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立淫羊藿提取物中残留有机溶剂:氯仿、乙酸乙酯、乙醇、正己烷、苯、甲苯、二甲苯、苯乙烯和二乙烯苯的检测方法。方法:采用静态顶空色谱法,用Agilent INNOWAX毛细管柱(30 m×0.320 mm,0.25μm)分离测定氯仿、乙酸乙酯、乙醇、正己烷、苯、甲苯、二甲苯、苯乙烯和二乙烯苯。以60℃为起始柱温,保持5 min,再以5℃·min^(-1)升至120℃,保持2 min,最后以15℃·min^(-1)升至180℃,保持3 min,使用氢火焰离子检测器。结果:9种残留溶剂在26 min内能很好地分离;标准曲线线性良好,r均≥0.9927,残留溶剂的回收率在82.26%～117.00%之间,RSD<10.32%;精密度<9.80%;9种有机溶剂的检测限范围为0.00001706%～0.004890%。淫羊藿提取物中仅检测到乙酸乙酯和乙醇,其含量都低于0.15%,而正己烷、氯仿、苯、甲苯、二甲苯、苯乙烯和二乙烯苯在样品中未检出。结论:本实验建立的方法能有效检测淫羊藿提取物中9种残留有机溶剂,待测样品中残留有机溶剂含量符合中国药典规定。Objective ： To establish a method of headspace capillary gas chromatography for the detection of residual solvents, including chloroform,ethyl acetate,hexane, ethanol, benzene, methyl benzene, dimethyl benzene, benzene vinyl and divinyl - benzene in extracts of Herba Epimedii. Methods： The nine residual solvents were separated by Agilent INNOWAX capillary column （30 m ×0. 320 mm, 0. 25 μm） with an FID detector. The carried gas was nitrogen. The column temperature was programmed from 60 ℃ （5 min isothermal） to 120 ℃ at a rate of 5 ℃ ·min^-1 , holding 2 min, then raised to 180 ℃ with a rate of 15 ℃ ·min^-1, this finished temperature was maintained for 3 min. Results ： All the nine residual solvents were well separated in 26 minutes. The recoveries of residual solvents were between 82.26% - 117.00% , with RSD less than 10. 32% （n = 3）. The night solvents＇ limits of detection were among 0. 00001706% -0. 004890%. Only ethyl acetate and ethanol were detected in the extracts of Herba Epimedii, and the contents are all lower than 0. 15%. Conclusion：The established method can be used for the detection of residual solvents in Extracts of Herba Epimedii, and the contents of these residual solvents are all meet the standards of ChP.

关 键 词：顶空气相色谱法 淫羊藿提取物 残留有机溶剂 

分 类 号：R917[医药卫生—药物分析学]