分散固相萃取/高效液相色谱-串联质谱法同时测定中药和保健食品中7种胰岛素分泌促进剂  

Simultaneous Determination of 7 Insulinotropic Agents in Traditional Chinese Medicines and Health Care Products by Dispersive Solid Phase Extraction-High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：朱明达[1,2,3] 陈冬东[1] 马微[1,3] 彭涛[1] 李晓娟[1] 李立[1] 代汉慧[1] 唐英章[1,3] 

机构地区：[1]中国检验检疫科学研究院,北京100025 [2]内蒙古工业大学,呼和浩特010051 [3]中国农业大学食品科学与营养工程学院,北京100083

出　　处：《分析化学》2011年第2期213-218,共6页Chinese Journal of Analytical Chemistry

基　　金："十一五"国家科技支撑计划项目(No.2006BAD27B02);国家质量监督检验检疫总局科技计划项目(No.2009IK323)资助

摘　　要：建立了测定中药和保健食品中7种非法添加胰岛素分泌促进剂(甲苯磺丁脲、妥拉磺脲、格列吡嗪、格列齐特、格列本脲、格列美脲、格列喹酮)的高效液相色谱-串联质谱分析方法。不同样品经含有0.1%甲酸的甲醇混合液提取后,采用C18吸附剂分散固相萃取后冷冻离心,得到样品溶液,以CAPCELL PAK C18 MGⅢ柱(100 mm×2.0 mm,5!m)分离,采用HPLC-MS/MS电喷雾电离(ESI),多反应监测(MRM)模式检测,以保留时间和子离子比定性,外标法定量。7种胰岛素分泌促进剂的检出限为0.1～0.3 mg/kg,定量限为0.3～0.9 mg/kg;在低、中、高的3个添加水平范围内的平均回收率为82.4%～105.3%;日内精密度均小于12%,日间精密度均小于15%。本方法分析速度快,灵敏度高,重现性好,可用于不同中药和保健食品中非法添加胰岛素分泌促进剂的检测。A comprehensive analytical method based on high performance liquid chromatography tandem mass spectrometry has been developed for the determination of 7 insulinotropic agents（Tolbutamide,Tolazamide,Glipizide,Gliclazide,Glibenclamide,Glimepiride and Glurenor）.Various samples were extracted under 0.1% formic acid-methanol.The sample extract was cleaned up respectively by C18 dispersive solid-phase extraction and freezing centrifugation.The 7 insulinotropic agents were separated on CAPCELL PAK C18 MGⅢcolumn（100 mm×2.0 mm,5 μm） and determined on HPLC-MS/MS by electrospray ionization（ESI） using multiple reaction monitoring（MRM）.Identification was achieved by the retention time and the ion ratio,quantification was done by the external standard curves.The limits of detection for the appetite suppressants were 0.3-0.9 mg/kg.The mean recoveries at the three spiked levels（low,middle and high） were 82.4%-105.3%,with the intra-day precision less than 12% and the inter-day precision less than 15%.The method is reliable,sensitive,and reproducible and adapts to the determination of the insulinotropic agents in different Traditional Chinese Medicines and health care products.

关 键 词：高效液相色谱-串联质谱 分散固相萃取 胰岛素分泌促进剂 

分 类 号：O657.63[理学—分析化学] R288[理学—化学] R155[医药卫生—中药学]