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

doi:10.3969/j.issn.1007-2861.2013.04.005

上海大学学报(自然科学版) ›› 2013, Vol. 19 ›› Issue (4): 354-357.doi: 10.3969/j.issn.1007-2861.2013.04.005

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

郑柯文1, 李寒1, 王昭1, 汪洋1, 鹿建霞1,
马盛韬2, 于志强2, 任国发1,2, 傅家谟1,2

(1. 上海大学环境与化学工程学院, 上海200444;2. 中国科学院广州地球化学研究所, 有机地球化学国家重点实验室, 广州510640)

出版日期:2013-08-27 发布日期:2013-08-27
作者简介:任国发(1979—), 男, 副研究员, 博士, 研究方向为持久性有机污染物. E-mail: rgf2008@shu.edu.cn
基金资助:
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)

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

ZHENG Ke-wen1, LI Han1, WANG Zhao1, WANG Yang1, LU Jian-xia1,
MA Sheng-tao2, YU Zhi-qiang2, REN Guo-fa1,2, FU Jia-mo1,2

(1. School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444, China;
(2. State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry,
Chinese Academy of Sciences, Guangzhou 510640, China)

Online:2013-08-27 Published:2013-08-27

摘要/Abstract

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.

关键词: 甲基三氯生, 气相色谱/质谱, 三氯生, 鱼肉样品

Abstract: 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.

Key words: gas chromatography/mass spectrometry (GC/MS);fish samples, methyl-triclosan (MTCS), triclosan (TCS)

中图分类号:

TU 411

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.

参考文献

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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

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