Institute of Analytical and Applied Chemistry, Department of Chemistry, Zhejiang University, Hangzhou, 310027, China.
Anal Chim Acta. 2013 Sep 24;796:7-13. doi: 10.1016/j.aca.2013.08.017. Epub 2013 Aug 14.
This work demonstrated the feasibility of mercury speciation analysis by anion exchange chromatographic separation with inductively coupled plasma mass spectrometry detection. For the first time, by complexing with the mobile phase containing 3-mercapto-1-propanesulfonate into negatively charged complexes, fast separation of inorganic mercury (Hg(2+)), monomethylmercury (MeHg), ethylmercury (EtHg) and phenylmercury (PhHg) was achieved within 5 min on a 12.5-mm strong anion exchange column. The detection limits for Hg(2+), MeHg, EtHg and PhHg were 0.008, 0.024, 0.029 and 0.034 μg L(-1), respectively. The relative standard deviations of peak height and peak area (5.0 μg L(-1) for each Hg species) were all below 3%. The determined contents of Hg(2+), MeHg and total Hg in a certified reference material of fish tissue by the proposed method were in good accordance with the certified values with satisfactory recoveries. The relative errors for determining MeHg and total mercury were -2.4% and -1.2%, respectively, with an acceptable range for spike recoveries of 94-101%. Mercury speciation in 11 fish samples were then analyzed after the pretreated procedure. The mercury contents in all fish samples analyzed were found compliant with the criteria of the National Standards of China.
本文展示了通过阴离子交换色谱分离与电感耦合等离子体质谱检测相结合进行汞形态分析的可行性。首次通过与含有 3-巯基-1-丙磺酸盐的流动相形成带负电荷的配合物，在 12.5mm 强阴离子交换柱上，可在 5 分钟内实现无机汞 (Hg(2+))、甲基汞 (MeHg)、乙基汞 (EtHg) 和苯基汞 (PhHg) 的快速分离。Hg(2+)、MeHg、EtHg 和 PhHg 的检测限分别为 0.008、0.024、0.029 和 0.034μg L(-1)。每个 Hg 物种 5.0μg L(-1)时，峰高和峰面积的相对标准偏差均低于 3%。采用所提出的方法测定鱼组织标准物质中 Hg(2+)、MeHg 和总 Hg 的含量与认证值吻合良好，回收率令人满意。测定 MeHg 和总汞的相对误差分别为-2.4%和-1.2%，加标回收率的可接受范围为 94-101%。然后对 11 个鱼样进行了预处理后进行汞形态分析。所有分析鱼样中的汞含量均符合中国国家标准的要求。
