顶空气相色谱法测定苦参总碱中三氯甲烷的残留量  

Headspace GC determination of residual chloroform in matrine

作　　者：贺凯 王汉卿[2] 王坤 王英华 

机构地区：[1]宁夏回族自治区药品检验所,银川750004 [2]宁夏医科大学药学院,银川750004

出　　处：《药物分析杂志》2011年第9期1824-1826,共3页Chinese Journal of Pharmaceutical Analysis

基　　金：宁夏十一五科技攻关项目;宁科技字[2006]74号

摘　　要：目的:建立苦参总碱中三氯甲烷残留的检测方法。方法:采用气相色谱顶空进样法,聚乙二醇(DB-WAX)毛细管柱,FID检测器,柱温采用程序升温,初始温度为60℃,保持6 min,然后以15℃.min-1升温速率升至180℃,保持5 min。结果:各个峰的分离效果好,三氯甲烷浓度在12.4～1236.6μg.mL-1的范围内呈良好的线性关系(r=0.9940),平均回收率为94.5%。结论:本方法结果准确、灵敏度高、重复性好,可以作为苦参总碱中三氯甲烷残留的检测方法。Objective：To establish a method to determine the residual chloroform in matrine.Methods：Using DB-WAX capillary column,FID detector and program temperature.The initial temperature was kept at 60 ℃ for 6 minutes,then the temperature was raised to 180 ℃ at the rate of 15 ℃·min-1 and kept for 5 minutes.Results：All the peaks were completely separated,the calibration curve showed a good linearity with the range of 12.4-1236.6 μg·mL-1（r=0.9940）.The average recovery was 94.5%.Conclusion：The method is accurate,sensitive and repetitive to determine residual chloroform in matrine.

关 键 词：原料药 生物碱 苦参总碱 三氯甲烷残留 残留溶剂 顶空气相色谱法 

分 类 号：R917[医药卫生—药物分析学]