Division of Earth and Environmental science, Graduate School of Science and Engineering, Kagoshima University, 1-21-35 Korimoto, Kagoshima 890-0065, Japan.
J Chromatogr A. 2013 May 3;1288:155-9. doi: 10.1016/j.chroma.2013.02.004. Epub 2013 Feb 8.
A method for the simultaneous determination of monomethylmercury (MeHg(+)) and monoethylmercury (EtHg(+)) in soil/sediment samples was developed. The method involves eluting mercury species from the soil/sediment samples using 5M HCl containing 5mM Pd(2+) and 0.1M Cu(2+) and then extracting MeHg(+) and EtHg(+) into toluene as chlorides. These alkylmercury chlorides are then back-extracted into an aqueous EDTA solution, creating EDTA complexes. Finally, an emetine-dithiocarbamate (emetineCS2) solution is added to the EDTA solution to form emetineCS2-alkylmercury complexes. EmetineCS2-MeHg and emetineCS2-EtHg were separated using reverse-phase HPLC and then detected by the chemiluminescence reaction with tris(2,2'-bipyridine)ruthenium(III). The MeHg(+) and EtHg(+) calibration curves, using the peak height, were linear from 0.5 to 20ng (as Hg). The detection limit was 0.16ng/g (analyzing 1g soil or sediment). The procedure was validated by analyzing a certified reference material (ERM CC580, estuarine sediment). The MeHg(+) concentration determined using the proposed method was in good agreement with the certified value, and EtHg(+) was detected in the reference material. A preliminary study of the relationship between environmental mercury concentrations and MeHg(+) production was performed.
一种同时测定土壤/沉积物样品中一甲基汞（MeHg(+)）和一乙基汞（EtHg(+)）的方法被开发出来。该方法涉及使用含有 5mM Pd(2+)和 0.1M Cu(2+)的 5M HCl 从土壤/沉积物样品中洗脱汞物种，然后将 MeHg(+)和 EtHg(+)作为氯化物提取到甲苯中。这些烷基汞氯化物随后被反萃取到含有 EDTA 的水溶液中，形成 EDTA 络合物。最后，将吐根碱-二硫代氨基甲酸盐（emetineCS2）溶液加入到 EDTA 溶液中，形成 emetineCS2-烷基汞络合物。使用反相 HPLC 将 emetineCS2-MeHg 和 emetineCS2-EtHg 分离，然后通过与三（2,2'-联吡啶）钌（III）的化学发光反应进行检测。使用峰高，MeHg(+)和 EtHg(+)的校准曲线在 0.5 到 20ng（作为 Hg）之间呈线性。检测限为 0.16ng/g（分析 1g 土壤或沉积物）。通过分析认证参考物质（ERM CC580，河口沉积物）验证了该程序。使用所提出的方法确定的 MeHg(+)浓度与认证值吻合良好，并且在参考物质中检测到了 EtHg(+)。还进行了环境汞浓度与 MeHg(+)生成之间关系的初步研究。
