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
查看参考文献10篇
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文摘
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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. |
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其他语种文摘
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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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来源
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上海大学学报. 自然科学版
,2013,19(4):354-357,367 【扩展库】
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关键词
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三氯生
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甲基三氯生
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气相色谱/质谱
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鱼肉样品
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地址
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1.
上海大学环境与化学工程学院, 上海, 200444
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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
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上海大学环境与化学工程学院, 有机地球化学国家重点实验室, 上海, 200444
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语种
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中文 |
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文献类型
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研究性论文 |
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ISSN
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1007-2861 |
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学科
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建筑科学 |
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基金
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国家自然科学基金
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国家重大科技专项子课题资助项目
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上海市重点学科建设项目
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文献收藏号
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CSCD:4942855
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参考文献 共
10
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