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食品研究与开发:2016,37(1):145-148
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P&T-GC-CVAFS法测定海产动物中的甲基汞和乙基汞
崔颖,肖亚兵,王禹,高健会
(天津出入境检验检疫局 动植物与食品检测中心,天津 300461)
Purge and Trap Gas Chromatography-Cold Vapor Atomic Fluorescence Spectrometry Determination of Methyl Mercury and Ethyl Mercury in Marine Animals
CUI Ying, XIAO Ya-bing, WANG Yu, GAO Jian-hui
(Animal, Plant and Foodstuffs Inspection Center, Tianjin Entry-exit Inspection and Quarantine Bureau,Tianjin 300461, China)
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投稿时间:2015-09-01    
中文摘要: 海产动物样品经过 30 %硝酸溶液提取,用 2 mol/L 醋酸钠-醋酸缓冲溶液调节 pH 后,用吹扫捕集-气相色谱冷原子荧光光谱仪联用系统测定其中的甲基汞和乙基汞的含量。使用衍生试剂,将甲基汞转化为甲基丙基汞,乙基汞转 化为乙基丙基汞,吹扫捕集进行富集并进一步消除基体干扰。以空白样品为基体,添加 3 种浓度水平的甲基汞和乙基汞 标准溶液,测得甲基汞的回收率为 80.5 %~103.2 %,相对标准偏差(n=6)为 1.7 %~6.9 %;乙基汞的回收率在 84.2 %~103.7 %, 相对标准偏差(n=6)为 2.3 %~7.0 %。
Abstract:Marine animals sample was extracted with 30 % nitric acid solution, and then adjusted the pH with 2 mol/L sodium acetate-acetic acid buffer solution. The eluate obtained was determined and identified by purge and trap gas chromatography -cold vapor atomic fluorescence spectrometry (P&T -GC -CVAFS). The propylation derivatization converted Methyl mercury (MeHg) to the more volatile methyl propyl mercury (MeHgPr), Ethyl mercury(EtHg) to the more volatile ethyl propyl mercury(EtHgPr), which could be concentrated through purge and trap system with a further clean-up of matrix. Tests for recovery were made by addition of standard MeHg and EtHg solutions at 3 different concentration levels to blank marine animals sample matrixes, values of MeHg recovery found were in the range from 80.5 % to 103.2 %, with RSDs (n=6) in the range from 1.7 % to 6.9 %; values of EtHg recovery found were in the range from 84.2 % to 103.7 %, with RSDs(n=6) in the range from 2.3 % to 7.0 %.
文章编号:201601034     中图分类号:    文献标志码:A
基金项目:天津出入境检验检疫局资助项目(TK077-2013)
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