摘要
采用气相色谱/质谱(gas chromatography/mass spectrometry,GC/MS)法,建立了可同时检测鱼肉样品中三氯生(triclosan,TCS)和甲基三氯生(methyl-triclosan,MTCS)的分析方法,对比了不同衍生化试剂的衍生效果,考察了对鱼肉样品去脂净化过程有影响的相关因素,最终确定鱼肉样品用正己烷-丙酮(体积比为1∶1)提取,凝胶色谱(gel permeation chromatography,GPC)和复合硅胶柱净化,乙酸乙酯衍生化,气相色谱/质谱检测.结果显示,本方法对TCS和MTCS的线性范围分别为5~500和2~500 pg/μL,相关系数均大于0.99,检出限(limit of detection,LOD)分别为1.3和0.8 pg/μL.在3个空白加标实验中,TCS和MTCS的回收率分别为83%~89%和85%~98%.最后,应用此方法对鱼肉样品中两种化合物的浓度进行了定量分析.
Gas chromatography coupled with mass spectrometry (GC/MS) was developed for the simultaneous determination of triclosan (TCS) and methyl-triclosan (MTCS) in fish samples. Parameters affecting both derivatization and clean-up procedures were studied. After extracting with hexane and actone (Vhexane : Vactone = 1 : 1), cleaning-up with gel permeation chromatography (GPC) and silica gel packed column, the residues were derivatized with acetic anhydride and analyzed by GC/MS. Under the optimal conditions, the linear range was 5- 500 pg/μL for TCS and 2-500 pg/μL for MTCS. The correlation coefficient R was above 0.99 for the analytes, with the limit of detection (LOD) 1.3 and 0.8 pg/μL, respectively. Good recoveries (83%-89% for TCS and 85%-98% for MTCS) were achieved in the spiking experiments. The established method was successfully applied to determine this analytes in real fish samples.
出处
《上海大学学报(自然科学版)》
CAS
CSCD
北大核心
2013年第4期354-357,367,共5页
Journal of Shanghai University:Natural Science Edition
基金
国家自然科学基金资助项目(21007037
41273121)
国家重大科技专项子课题资助项目(2009ZX07528-002-04)
上海市重点学科建设资助项目(S30109)
关键词
三氯生
甲基三氯生
气相色谱
质谱
鱼肉样品
triclosan (TCS)
methyl-triclosan (MTCS)
gas chromatography/mass spectrometry (GC/MS)
fish samples