微波辅助萃取法/高效液相色谱-串联质谱法对减肥保健食品中非法添加药物奥利司他的测定  

Determination of Illegal Drug Orlistat Added in the Weight-loss Functional Foods by Microwave Assisted Extraction/High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：马微[1,2] 付丽 王海波 陈伟[4] 王秀君[4] 于静[4] 唐英章[4] 

机构地区：[1]中国农业大学食品科学与营养工程学院,北京100083 [2]东宁出入境检验检疫局,黑龙江东宁157200 [3]郑州牧业工程高等学校,河南郑州450011 [4]中国检验检疫科学研究院,北京100123

出　　处：《分析测试学报》2009年第9期1045-1048,1053,共5页Journal of Instrumental Analysis

基　　金：国家科技支撑计划农业领域课题资助项目(2006BAD27B02)

摘　　要：建立了测定减肥保健食品中非法添加药物奥利司他的高效液相色谱-串联质谱分析方法。减肥保健食品经微波辅助萃取后,经Waters Atlantis T3柱(3μm,150mm×2.1mm)分离,采用多反应监测正离子模式检测,定性离子对为m/z496.3>319.2、m/z496.3>160.0,定量离子对为m/z496.3>160.0。结果表明,奥利司他的仪器检出限为0.2μg/L;在0.2～500μg/L范围内呈良好的线性关系,相关系数为0.9997。在低、中、高3个添加水平范围内的平均回收率为86%～104%;日内精密度均小于6%,日间精密度均小于8%。方法分析速度快、灵敏度高、重复性好,可用于不同减肥保健食品中非法添加奥利司他的快速检测。A comprehensive analytical method based on high performance liquid chromatography tan- dem mass spectrometry（ HPLC - MS/MS） has been developed for the determination of orlistat. Vari- ous weight-loss functional foods were extracted by microwave assisted extraction and separated on a Waters Atlantis T3（3μm, 150 mm x2. 1 mm） column. The detection of orlistat was performed by MS/MS using positive electrospray ionization and multiple reaction monitoring（MRM） mode, and se- lecting two precursor-product ion pairs： m/z 496. 3 〉 319. 2, m/z 496. 3 〉 160. 0 as qualitative ion pairs, and m/z 496. 3 〉 160. 0 as quantification ion pair. The result showed that the limit of detec- tion for orlistat was 0. 2 μg/L. The calibration curve showed a good linearity for orlistat in the con- centration ranges of 0.2 -500 μg/L with a correlative coefficient of 0. 999 7. The mean recoveries at the three spiked concentration levels（ low, middle, high） were between 86% and 104%. The intra- RSD was less than 6% and inter-RSD was less than 8% . The method is reliable, sensitive and re- producible, and could be rapidly applied in the determination of orlistat in different weight-loss func- tional foods.

关 键 词：高效液相色谱-串联质谱 微波辅助萃取 奥利司他 裂解途径 减肥保健食品 

分 类 号：O657.63[理学—分析化学] R927.2[理学—化学]