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
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)