血中甲基汞和无机汞的高效液相色谱-串联电感耦合等离子体质谱测定法

发布时间：2018-03-30 01:32

本文选题：血　切入点：甲基汞　出处：《环境与健康杂志》2017年01期

【摘要】：目的建立高效液相色谱-串联电感耦合等离子体质谱法(HPLC-ICP-MS)同时测定血中甲基汞和无机汞的方法。方法血样先加甲醇沉淀蛋白,再以含有0.05%(体积分数)2-巯基乙醇、3 g/L L-半胱氨酸和0.1%(体积分数)盐酸的溶液室温超声提取,样品中的甲基汞和无机汞经络合提取后,以含有5%(体积分数)甲醇、0.06 mol/L乙酸铵、0.05%(体积分数)2-巯基乙醇、3 g/L L-半胱氨酸的水溶液作为流动相,经C18液相色谱柱分离后,用ICP-MS No gas模式进行测定,外标法定量。结果甲基汞和无机汞分别在0.30~50μg/L和0.50~50μg/L的线性范围内,所得回归方程均呈较好的线性关系,r0.999。该方法对样品中甲基汞、无机汞的检出限分别为1、1.6μg/L,定量下限分别为3、5μg/L,平均回收率分别在91.5%~95.8%和92.1%~96.3%之间,RSD分别在2.63%~4.23%和2.12%~4.52%之间。结论该法需血量少、提取效率高、干扰小、定量准确,适用于甲基汞和无机汞的内暴露健康影响评价和急性中毒实验室诊断测定。
[Abstract]:Objective to establish a high performance liquid chromatography-tandem inductively coupled plasma mass spectrometry (HPLC-ICP-MS) method for simultaneous determination of methylmercury and inorganic mercury in blood. Then it was extracted by ultrasonic at room temperature in a solution containing 0.05% (volume fraction of 2-mercaptoethanol) 3 g / L L-cysteine and 0.1 (volume fraction) hydrochloric acid. After the meridian extraction of methylmercury and inorganic mercury in the sample, The mobile phase was composed of aqueous solution containing methanol 0.06 mol/L ammonium acetate and 2-mercaptoethanol 3 g / L L-cysteine. The mobile phase was separated by C18 liquid chromatographic column and determined by ICP-MS No gas mode. Results the linear range of methylmercury and inorganic mercury were in the range of 0.30 渭 g / L and 0.50 渭 g / L, respectively. The detection limit of inorganic mercury is 1 ~ 1.6 渭 g 路L ~ (-1), and the lower limit of quantification is 3 ~ 5 渭 g / L, respectively. The average recoveries of inorganic mercury are between 91.5 ~ 95.8% and 92.1% and 96.3%, respectively, and the RSD are between 2.63 ~ 4.23% and 2.12 ~ 4.52%. Conclusion the method has the advantages of low blood demand, high extraction efficiency, little interference and accurate quantification. It is suitable for health impact assessment of internal exposure to methylmercury and inorganic mercury and laboratory diagnosis of acute poisoning.
【作者单位】：上海市普陀区疾病预防控制中心理化检验科;
【基金】：上海市普陀区卫生系统自主创新科研资助项目(2015004)
【分类号】：O657.63;R446.1

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