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作 者:黄笑寒[1,2] 李玉锋[2] 董泽琴 李柏[2] 高愈希[2] 瞿丽雅 袁亚莉[1] 陈春英[2,4]
机构地区:[1]南华大学化学化工学院,衡阳421001 [2]中国科学院高能物理研究所多学科研究中心,北京100049 [3]贵州省环境科学研究设计院,贵阳550002 [4]国家纳米科学中心,北京100190
出 处:《分析试验室》2011年第7期14-17,共4页Chinese Journal of Analysis Laboratory
基 金:欧盟第六框架计划项目(FOOD-CT-2006-016253);国际原子能机构项目(15818);中国科学院重要方向性项目(KJCX3.SYW.N3);中国科学院高能物理研究所青年基金项目资助;贵州省科技厅社会发展攻关计划项目(黔科合[2010]3008与黔科合丁字[2007]2018)
摘 要:建立了反相色谱-氢化物发生原子荧光光谱联用测定血清中汞形态(无机汞和甲基汞)的方法,优化了载流液,还原剂以及2-巯基乙醇的浓度,以正辛醇作为消泡剂,成功地解决了测定血清样品时原子荧光仪器内气液分离器中产生大量泡沫的难题。采用反相色谱柱对无机汞和甲基汞形态进行了分离,回收率在95%~110%之间,无机汞和甲基汞的精密度RSD(n=7)分别为3.3%和4.0%,二者的检出限分别为0.28μg/L和0.11μg/L。当无机汞和甲基汞形态浓度范围为2~30μg/L时,两种形态均可得到良好的线性关系,线性相关系数均>0.9990。通过测定标准物质人发(GBW 07601)和鱼样(IAEA MA-B-3/TM)评价方法的可靠性。方法用于分析长期汞暴露地区人群口服补硒剂后血清中汞的化学形态并定量,结果发现硒能促进人体内汞的排出。A hyphenated technique of reversed phase(RP) chromatography and hydride generation atomic fluorescence spectrometry was established to determine mercury species(methylmercury and inorganic mercury) in serum from long-term mercury-exposed people supplemented with selenium.The concentration of carrier fluid,reducing agent,and 2-mercaptoethanol were optimized Octanol was used as a defoamer to solve the problem that lots of bubbles were generated in the gas-liquid separator of atomic fluorescence after sampling.The inorganic mercury and methylmercury were separated by using RP-column.The recoveries ranged between 95% and 110% and the RSD(n=7) and the detection limits of inorganic mercury and methylmercury were 3.3%,4.0% and 0.28 μg/L,0.11 μg/L,respectively.The inorganic mercury and methylmercury had good linear relationships with the concentrations of the two forms ranging from 2 to 30 μg/L and the linear correlation coefficients of standard curves R are more than 0.9990.The reliability of the method was evaluated by measuring the standard material of human hair(GBW 07601) and fish samples(IAEA MA-B-3/TM).This method is simple,fast,and sensitive and it was successfully applied to analysis of the mercury species in serum from long-term mercury-exposed people supplemented with selenium,it was found that selenium could promote the discharge of mercury from the body living in this area.
关 键 词:反相色谱 氢化物发生原子荧光光谱 无机汞 甲基汞
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