Chen Jianguo, Chen Hengwu, Jin Xianzhong, Chen Haiting
Department of Chemistry, Zhejiang University, Zijin'gang Campus, Hangzhou 310058, China.
Talanta. 2009 Feb 15;77(4):1381-7. doi: 10.1016/j.talanta.2008.09.021. Epub 2008 Sep 23.
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 degrees 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 Hg(2+), 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 Hg(2+), 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.
研究了在反相高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)检测联用之前,采用浊点萃取(CPE)对超痕量汞形态进行预富集的方法。甲基汞、乙基汞、苯基汞和无机汞等汞形态通过与二乙基二硫代氨基甲酸钠反应转化为疏水性螯合物,在40℃水浴加热时,疏水性螯合物被萃取到Triton X-114的富表面活性剂相中。发现乙基汞在CPE过程中部分分解,因此所建立的方法不包括乙基汞。对影响CPE预富集、HPLC分离和ICP-MS测定的各种实验条件进行了优化。在优化条件下,甲基汞离子、苯基汞离子和汞离子(Hg²⁺)的检出限分别为13、8和6 ng l⁻¹(以Hg计)。对含有三种汞形态且每种浓度均为0.5 ng ml⁻¹的标准溶液进行七次测定,甲基汞离子、苯基汞离子和汞离子(Hg²⁺)的相对标准偏差分别为5.3%、2.3%和4.4%。所建立的方法成功应用于环境水样以及人发和海洋鱼类等生物样品中三种汞形态的测定。