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《微波萃取液相色谱-电感耦合等离子体质谱联用测定水产品中甲基汞、乙基汞和无机汞.pdf》由会员上传分享,免费在线阅读,更多相关内容在应用文档-天天文库。
1、安徽农业科学,JournalofAnhuiAgri.Sci.2014,42(8):2438—2440责任编辑黄小燕责任校对况玲玲微波萃取液相色谱一电感耦合等离子体质谱联用测定水产品中甲基汞、乙基汞和无机汞王贤波,刘军波,余霞奎,钱丽华(杭州市农业科学研究院实验中心,浙江杭州310024)摘要[目的]研究水产品中甲基汞、乙基汞和无机汞的检测方法。[方法]采用Hypersilgold150x4.6mm色谱柱进行HPLC分离条件优化,用含Lj、co、In、u各1./L的调谐液进行ICP—MS参数优化,对样品进行微波萃取。[结果]采用盐酸微波萃取样品,c柱(150x4.6mm)分离,流动相为5%甲
2、醇一0.06mol/L乙酸铵~1L半胱氨酸。甲基汞、乙基汞的线性范围均为O.5~100.0gVL,检出限分别为0.2、0.3g/L;无机汞线性范围均为0.5~20.0g/L,检出限为0.2L。不同浓度下甲基汞、乙基汞、无机汞的加标回收率分别为89%~98%、82%~89%、86%~96%。鱼肉标准物质(GBW10029)中汞形态的测定均值在标准值范围内。I结论1该方法前处理简便、精密度高、准确性好,适用于水产品中汞化合物的形态分析。关键词微波萃取;液相色谱一电感耦合等离子体质谱;甲基汞;乙基汞;无机汞中图分类号S181.3文献标识码A文章编号0517—6611(2014)08—02438—
3、03SimultaneousDeterminationoftheContentofMethylMercury,EthylMercuryandInorganicMercuryinMicrowaveExtractionofA-qnaticProductsbyHPLC-ICP-MSWANGXial1.b0etal(LaI)0ratorialCenter,HangzhouInstituteofAculturalSciences,Hangzhou,Zhejiang310024)Abstract[Objectivei
4、r0observethedetectionmethodofmethylmercury
5、(MMC),ethyImercury(EMC)andinorganicmercury(MC)ina.quaticproducts.[Method]UsingHypersilgold150×4.6mmchromatographiccolumnforoptimizationofHPLCseparationconditions,.rheICP—MsparameteroptimizationusingtunedliquidcontainingLi,co,In,ulL,Thesampleswereextractedbymicrowave-[Result]Thesamplewasextractedwi
6、tl1hydrochloricacidandseparatedonaCfchromatographiccolumn(150×4.6mm)using5%methanol.06moL/Lammoniumacetate.1Lcysteineasmobilephase.Thelinearrangesformethylmercuryandethylmercurywereallbetween0and100LLLththedetection1imits0.2¨Land0.3“g/L.The1inearrangesforinorganicmereurywas0and20¨g/Lwiththedetecti
7、on1irnits0.2lJ.rhespikedrecoveriesfordifierentconcentrationsofmercurycompoundswereintherangeof89%一98%forMMC,82%一89%forEMCand86%.96%forMC.Themethodwasappliedinthedeterminationofmercuryspeciationsinfishreferencematerial(GBW1oo291andtheana—lyticalresultwasinthescopeofstandardvalue.IConclusionlI1}Iere
8、sultsindicatedthatthemethodhadasimplepre—treatmentprocedure.goodaccuracyandprecision,andwassuitableforthedeterminationofmercuryspeciationsinaquaticproducts.KeywordsMierowaveextraction:HPLC—ICP—MS:Methylmercury:Et
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