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.
郑柯文, 李寒, 王昭, 汪洋, 鹿建霞,马盛韬, 于志强, 任国发, 傅家谟
. 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[J]. 上海大学学报(自然科学版), 2013
, 19(4)
: 354
-357
.
DOI: 10.3969/j.issn.1007-2861.2013.04.005
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.
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