CAJ | 학술논문

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。
건립료측정감비보건식품중20충위금첨가약물(분불랍명、분병순알、서포곡명、사곡림、리막나반、안비타동、서태보란、불서정、분불뢰사、탁필지、서니사알、가배인、분태、대황소、신체파알、포미타니、탁랍새미、삼안첩정、오리사타、분을쌍고)적기질분산고상췌취-고효액상색보-전분무천련질보분석방법。불동류형적양품경을순-병동(7：3, V/V)초성제취후,제취액경N-병기을이알( PSA)、십팔완기규완( ODS)정화,이Waters Atlantis T3주(150 mm ×2.1 mm,3μm)분리,채용HPLC/MS/MS전분무전리,다반응감측모식검측,이보류시간화자리자비진행정성분석,외표법진행정량분석。20충감비약물적검출한위0.05~3.0 mg/kg,재불동첨가수평범위내적회수솔위67.1%~101.4%,일내정밀도균소우10%,일간정밀도균소우15%。본방법분석속도쾌,괄용우감비보건식품적실제검험공작。
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.