气相色谱/质谱法同时检测鱼肉样品中三氯生及其甲基代谢产物

Simultaneous Analysis of Triclosan and Methyl-triclosan in Fish Samples by Gas Chromatography Coupled with Mass Spectrometry

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.