Determination of ultra-trace amount methyl-, phenyl- and inorganic mercury in environmental and biological samples by liquid chromatography with inductively coupled plasma mass spectrometry after cloud point extraction preconcentration |
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Authors: | Jianguo Chen Hengwu Chen Xianzhong Jin |
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Affiliation: | a Department of Chemistry, Zhejiang University, Zijin’gang Campus, Hangzhou 310058, China b Ningbo Entry-exit Inspection and Quarantine Bureau, Ningbo 315012, China |
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Abstract: | The cloud point extraction (CPE) preconcentration of ultra-trace amount of mercury species prior to reverse-phase high performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP-MS) detection was studied. Mercury species including methyl-, ethyl-, phenyl- and inorganic mercury were transformed into hydrophobic chelates by reaction with sodium diethyldithiocarbamate, and the hydrophobic chelates were extracted into a surfactant-rich phase of Triton X-114 upon heating in a water bath at 40 °C. Ethylmercury was found partially decomposed during the CPE process, and was not included in the developed method. Various experimental conditions affecting the CPE preconcentration, HPLC separation, and ICP-MS determination were optimized. Under the optimized conditions, detection limits of 13, 8 and 6 ng l−1 (as Hg) were achieved for MeHg+, PhHg+ and Hg2+, respectively. Seven determinations of a standard solution containing the three mercury species each at 0.5 ng ml−1 level produced relative standard deviations of 5.3, 2.3 and 4.4% for MeHg+, PhHg+ and Hg2+, respectively. The developed method was successfully applied for the determination of the three mercury species in environmental water samples and biological samples of human hair and ocean fish. |
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Keywords: | Cloud point extraction Mercury speciation HPLC ICP-MS Water samples Biological samples |
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