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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

马微 程丽 张兰威 张英春 王海波 焦月华 代汉慧 唐英章

分析化学Issue(8):1162-1171,10.
分析化学Issue(8):1162-1171,10.DOI:10.11895/j.issn.0253-3820.140113

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 Dispersion-High Performance Liquid Chromatography Tandem Mass Spectrometry

马微 1程丽 2张兰威 3张英春 1王海波 1焦月华 4代汉慧 1唐英章5

作者信息

  • 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. 东宁出入境检验检疫局,东宁157200
  • 5. 中国检验检疫科学研究院,北京100123
  • 折叠

摘要

Abstract

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

Key words

High performance liquid chromatography tandem mass spectrometry/Matrix solid phase dispersion/Weight-loss functional foods/Mass spectrum fragmentation pathways

引用本文复制引用

马微,程丽,张兰威,张英春,王海波,焦月华,代汉慧,唐英章..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[J].分析化学,2014,(8):1162-1171,10.

基金项目

本文系国家质检总局科技计划基金(No.2013IK155)和国家自然科学基金(No.31101288)资助@@@@This work was supported by the General Administration of Quality Supervision, Inspection and Quarantine Science Foundation (No.2013IK155), and the National Natural Science Foundation of China (No.31101288) (No.2013IK155)

分析化学

OA北大核心CSCDCSTPCD

0253-3820

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