微波辅助萃取-液相色谱-原子荧光光谱法分析汞接触人群尿液中汞的形态  

Morphological analysis of mercury in urine of mercury exposed population by microwave-assisted extraction-liquid chromatography-atomic fluorescence spectrometry

作　　者：柯宗枝[1] 万玲利 姜志鹏 陈珊 陈进国[1] 

机构地区：[1]福建省职业病与化学中毒预防控制中心,福建福州350001

出　　处：《中国卫生检验杂志》2017年第24期3519-3522,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立汞接触人群尿液中无机汞(Hg)、甲基汞(Me Hg)和乙基汞(Et Hg)的微波辅助萃取-液相色谱-原子荧光光谱测定方法。方法取尿液样品5.0 ml,加入1.0 ml的6 mol/L盐酸后室温微波提取30 min,在冷水浴中用氨水调p H值至4.0,用流动相定容至10.0 ml,经0.45μm滤膜过滤,以5%甲醇溶液+3.8 g/L乙酸铵+1.0 g/L L-半胱氨酸作液相色谱流动相,经HG-C18柱分离,紫外消解后原子荧光光谱仪测定。结果无机汞、甲基汞和乙基汞在1.0μg/L^50.0μg/L呈良好的线性关系,相关系数r均>0.999,检出限分别为0.4μg/L、0.3μg/L、0.4μg/L,相对标准偏差RSD为1.50%~3.66%(n=6),回收率为91.3%~101.5%,样品在4℃可保存5 d。结论该方法分析速度快、灵敏度高、准确性好,适用于汞接触人群尿液中无机汞、甲基汞和乙基汞的同时测定。Objective To establish a method for the determination of mercury,methylmercury and ethylmercury in urine of mercury exposed population by microwave-assisted extraction-liquid chromatography-atomic fluorescence spectrometry. Methods 5 ml urine sample was extracted with 1. 0 ml of 6 mol/L Hcl at room temperature for 30 minutes. p H of the sample was adjusted to 4. 0 using ammonia water in cold water bath. The sample was fixed to 10 ml in mobile phase and filtered by 0. 45 μm membrane. The mobile phase of liquid chromatography was composed of 5% methanol solution ＋ 3. 8 g/L ammonium acetate ＋ 1. 0 g/L L-cysteine. The sample was separated on a HG-C18 column and detected by AFS after UV digestion. Results The method had a good linear relationship in range of 1. 0 μg/L-50. 0 μg/L,and the linear correlation coefficients were all greater than 0. 999 for three mercury species. The detection limits of Hg,Me Hg and Et Hg were 0. 5 g/L,0. 3 g/L and 0. 5 g/L respectively,with relative standard deviation（ RSD） within 1. 50%-3. 66%（ n = 6） and the average recovery rate of within 91. 3%-101. 5%. The sample can be stored for 5 d at 4 ℃. Conclusion The developed method is fast,sensitive and accurate. It is suitable for the simultaneous determination of mercury,methylmercury and ethylmercury in urine of mercury exposed population.

关 键 词：液相色谱-原子荧光 尿液 无机汞 甲基汞 乙基汞 汞接触人群 

分 类 号：O657[理学—分析化学]