基质分散固相萃取-高效液相色谱-串联质谱法同时测定减肥保健食品中20种违禁添加药物  

Simultaneous Determination of 20 Anti-Obesity Drugs Illegally Added in Weight-loss Functional Foods by Matrix Solid Phase DispersionHigh Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：马微[1,2] 程丽[3] 张兰威[1] 张英春[1] 王海波 焦月华[1] 代汉慧[4] 唐英章[4] 

机构地区：[1]哈尔滨工业大学,哈尔滨150001 [2]东宁出入境检验检疫局,东宁157200 [3]黑龙江大学,哈尔滨150080 [4]中国检验检疫科学研究院,北京100123

出　　处：《分析化学》2014年第8期1161-1170,共10页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局科技计划基金(No.2013IK155);国家自然科学基金(No.31101288)资助~~

摘　　要：建立了测定减肥保健食品中20种违禁添加药物（芬氟拉明、苯丙醇胺、西布曲明、舍曲林、利莫那班、安非他酮、西酞普兰、氟西汀、苯氟雷司、托吡酯、唑尼沙胺、咖啡因、酚酞、大黄素、吲达帕胺、布美他尼、托拉塞米、三氨喋啶、奥利司他、苯乙双胍）的基质分散固相萃取-高效液相色谱-电喷雾串联质谱分析方法。不同类型的样品经乙醇-丙酮（7∶3,V/V）超声提取后,提取液经N-丙基乙二胺（PSA）、十八烷基硅烷（ODS）净化,以Waters Atlantis T3柱（150 mm×2.1 mm,3μm）分离,采用HPLC/MS/MS电喷雾电离,多反应监测模式检测,以保留时间和子离子比进行定性分析,外标法进行定量分析。20种减肥药物的检出限为0.05~3.0 mg/kg,在不同添加水平范围内的回收率为67.1%~101.4%,日内精密度均小于10%,日间精密度均小于15%。本方法分析速度快,适用于减肥保健食品的实际检验工作。An analytical method based on high performance liquid chromatography tandem mass spectrometry has been developed for the simultaneous determination of 20 anti-obesity drugs （ fenfluramine, phenylpropanolamine, sibutramine, sertraline, rimonabant, bupropion, citalopram, fluoxetine, benfluorex, topiramate, zonisamide, caffeine, phenolphthalein, emodin, indapamide, bumetanide, torasemide, triamterene, orlistat, phenformin）. that were extracted from various weight-loss functional foods by ethanol-acetone（7：3, V/V）and purified by primary secondary amine （PSA） and octadecyltrimethoxysilane（ODS） under ultrasonication. The analysis was carried out on HPLC-MS /MS by electrospray ionization using multiple reaction monitoring after the chromatographic separation on Waters Atlantis T3 （3 μm, 150 mm × 2. 1 mm） column. Identification was achieved by the retention time and the ion ratio, quantification was done by the external standard method. The limits of detection for the appetite suppressants were 0. 05-3. 0 mg/kg. The mean recoveries at the three spiked levels were 67 . 1%-101 . 4%, with the intra-day precision less than 10%and the inter-day precision less than 15%. The method is reliable, accurate, reproducible and suitable for the determination of the anti-obesity drugs in different weight-loss functional foods.

关 键 词：高效液相色谱-串联质谱 基质分散固相萃取 减肥保健食品 质谱裂解途径 

分 类 号：O657.63[理学—分析化学] TS218[理学—化学]