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室温离子液体作溶剂顶空气-质联用测定药物中溶剂残留
引用本文:江海亮,沈昊宇,乐长高,周赛春.室温离子液体作溶剂顶空气-质联用测定药物中溶剂残留[J].分析化学,2006,34(7):1027-1029.
作者姓名:江海亮  沈昊宇  乐长高  周赛春
作者单位:1. 浙江大学宁波理工学院分析测试中心,宁波,315100
2. 东华理工学院应用化学系,抚州,344000
基金项目:国家自然科学基金;浙江省分析测试基金;宁波理工学院校科研和教改项目
摘    要:基于室温离子液体无蒸汽压、良好溶解性和分散性的特点,用室温离子液体bm im]PF6]作溶剂顶空气-质联用测定非那雄胺中二氯甲烷、三氯甲烷及二氧六环的残留量,优化了顶空气-质联用分析条件。二氯甲烷、三氯甲烷及二氧六环的检出限分别为0.2、0.02和0.50 ng,线性相关系数大于0.99;相对标准偏差(RSD)0.39%~4.60%;回收率为90.5%~111.9%。室温离子液体作为顶空溶剂的灵敏度有所提高。

关 键 词:室温离子液体  非那雄胺  溶剂残留  [bmim][PF6]  顶空气-质联用
收稿时间:05 26 2005 12:00AM
修稿时间:2005-05-262005-07-25

Room Temperature Ionic Liquid as a Novel Medium for the Determination of Solvent Residuals in Drug with Headspace Gas Chromatography-Mass Spectrometry
Jiang Hailiang,Shen Haoyu,Le Zhanggao,Zhou Saichun.Room Temperature Ionic Liquid as a Novel Medium for the Determination of Solvent Residuals in Drug with Headspace Gas Chromatography-Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2006,34(7):1027-1029.
Authors:Jiang Hailiang  Shen Haoyu  Le Zhanggao  Zhou Saichun
Institution:1.Analysis and Testing Center, Ningbo Institute of Technology, Zhejiang University, Ningbo 315100; 2 . Department Applied Chemistry of East China Institute of Technology, Fuzhou 344000
Abstract:A typical room temperature ionic liquid,1-butyl-3-methylimidazolium hexafluoro-phosphate \\,was used as an alternative solvent to determine solvent residuals in drug with headspace gas chromatography mass detector(HS-GC-MS).Injection temperature,equilibrium time and chromatographic condition were optimized.The method was used for the detection of dichloromethane,trichloromethane and(dioxane) in Finasteride.The detection limits of dichoromethane,trichloromethane,dioxane were 0.2,0.02 and 0.50 ng,respectively,with linear correlation coefficients exceeding 0.99.The relative standard deviations(RSD) were less than 4.6%.The recoveries for dichoromethane,trichloromethane,dioxane were in the range of 90.5%-111.9%.The results showed that the sensitivity of dichoromethane,trichloromethane,(dioxane) obtained by \PF_(6) HS-GC-MS method over 5 times higher than those obtained by dimethylformamide(DMF) HS-GC-MS.
Keywords:Room temperature ionic liquids  1-butyl-3-methylimidazolium hexafluorophosphate  solvent(residuals)  finasteride  headspace gas chromatogrpahy-mass spectrometry  
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