高效液相色谱与原子荧光光谱联用分析海产品中的甲基汞  

Determination of methylmecury in seafood using high performance liquid chromatography coupled with atomic fluorescence spectrometry

作　　者：刘庆阳[1,2] 何滨[2] 胡敬田[1] 江桂斌[2] 

机构地区：[1]山东大学环境研究院,济南250100 [2]中国科学院生态环境研究中心,环境化学与生态毒理学国家重点实验室,北京100085

出　　处：《分析试验室》2009年第5期41-44,共4页Chinese Journal of Analysis Laboratory

基　　金：国家科技支撑计划科学仪器设备研制与开发(2006BAK03A14)项目资助

摘　　要：建立了高效液相色谱-紫外消解-氢化物发生-原子荧光光谱联用测定海产品中甲基汞的方法,比较了不同溶剂对海产品中甲基汞提取效率的影响。实验采用质量分数25%(m/V)KOH甲醇溶液,室温振荡10 h消解样品,CH2Cl2萃取,再以0.01 mol/L Na2S2O3水溶液反萃取,并采用HPLC-UV-HG-AFS测定鱼和扇贝萃取液中的甲基汞的含量。在优化分离和前处理条件下,平行进样5次10 ng/mL的汞混合标准溶液,甲基汞、无机汞和乙基汞的色谱峰面积的相对标准偏差(RSDs)分别为4.4%、3.9%和4.3%,甲基汞、无机汞和乙基汞的检出限分别为0.069、0.15和0.046 ng/mL;鱼和扇贝的甲基汞的加标回收率为96±5%和95±5%。A method based on high performance liquid chromatography-UV-hydride generation on line coupled with atomic fluorescence spectrometry （HPLC-UV-HG-AFS） for mercury speciation in seafood was proposed. Different extraction methods for methylmecury in fish and shellfish were also investigated. The samples were digested by 25% KOH in methanol, shaken for 10 hours, extracted by CH2Cl2, subsequently back-extracted by 0.01mol/L Na2S2O3 and then measured. Under the optimized conditions, the relative standard deviations for the determination of methyl-, inorganic and ethylmercury were 4.4%, 3.9% and 4.3%, the detection limits for methyl-, inorganic and ethylmercury were 0.069, 0.15 and 0.046 ng/mL respectively. The recoveries for methylmercury in fish and shellfish were 96±5% and 95±5%.

关 键 词：高效液相色谱 紫外消解 氢化物发生 原子荧光联用系统 海产品 汞 形态分析 

分 类 号：O557.3[理学—热学与物质分子运动论] O657.7[理学—物理]