Mercury speciation by liquid chromatography coupled with on-line chemical vapour generation and atomic fluorescence spectrometric detection (LC-CVGAFS).
Mercury speciation by liquid chromatography coupled with on-line chemical vapour generation and atomic fluorescence spectrometric detection (LC-CVGAFS).
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DOI：
10.1016/j.talanta.2004.12.031
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发表时间：
2005-04
期刊：
影响因子：
6.1
通讯作者：
E. Bramanti;Cristina Lomonte;M. Onor;R. Zamboni;A. D’Ulivo;G. Raspi
中科院分区：
文献类型：
--
作者：
E. Bramanti;Cristina Lomonte;M. Onor;R. Zamboni;A. D’Ulivo;G. Raspi
提出了反相色谱(RPC)与紫外-可见二极管阵列检测器(DAD)和冷原子荧光光谱分析(CVGAFS)在线联用的方法，用于半胱氨酸、青霉胺和谷胱甘肽络合物中无机汞和有机汞(甲基汞、乙基汞和苯基汞)的形态和测定。汞-硫醇络合物在C18反相柱上分离，在HCl介质中由KBrR/KBrO_3产生的溴在线氧化，以便在室温下在30 cm的针织线圈中在2.5s内将有机汞物种快速转化为无机汞。在Ar/H_2小型化火焰中，氢化钠还原为Hg0后，用原子荧光光谱仪选择性地检测到Hg(II)。在最佳条件下，在线溴处理对无机汞的回收率分别为79%~85%、80%~85%、63%~76%，具体取决于采用的络合硫醇。给出了三种络合剂的最佳洗脱条件。在优化的条件下，无机汞、甲基汞、乙基汞和苯基汞的检出限分别为16、18、18和20pg(以汞计)，相对标准偏差(R.S.D)在1.5%~2.0%之间，进样动态范围为0.1~100 ng。通过对DORM-2和NIES CRM 13两种证书标准物质的分析，验证了LC-DAD-CVGAFS方法的有效性，甲基汞的回收率分别为98±6%和97±5%。
Reverse phase chromatography (RPC) coupled on-line with UV–vis diode array detector (DAD) and cold vapour generation atomic fluorescence spectrometry (CVGAFS) is proposed for the speciation and determination of inorganic and organic mercury (methylmercury, ethylmercury and phenylmercury) in the form of cysteine, penicillamine and glutathione complexes. The mercury–thiol complexes are separated on a C18Reverse Phase column and oxidized on-line with bromine, generated in situ by KBr/KBrO3in HCl medium, in order to fast convert organic mercury species to inorganic mercury in less than 2.5s, at room temperature, in a 30cm knitted coil. Hg(II) is selectively detected by AFS in a Ar/H2miniaturized flame after sodium borohydride reduction to Hg0. Under optimized conditions, on-line bromine treatment gives recoveries of thiol-complexed methylmercury, ethylmercury and phenylmercury with respect to inorganic mercury ranging between 79 and 85%, 80 and 85%, 63 and 76%, respectively, depending on the complexing thiol employed. Optimized elution conditions were provided in the three complexing agents. The detection limits (LODc) for inorganic mercury, methylmercury, ethylmercury and phenylmercury, in the optimized conditions complexed with thiols were about 16, 18, 18 and 20pg (as mercury), respectively, a relative standard deviation (R.S.D) ranging between 1.5 and 2.0%, and a linear dynamic range between 0.1 and 100ng injected. LC–DAD–CVGAFS method has been validated by analysing two certificate reference material, DORM-2 and NIES CRM 13, obtaining 98±6 and 97±5% of methylmercury recovered, respectively.