HPLC–ICP–MS法测定农田土壤中甲基汞和乙基汞

Determination of Merthyl Mercury and Ethyl Mercury in Field Soil by HPLC–ICP–MS

采用HPLC 反相C18 柱分离、ICP–MS 检测,建立了农田土壤中甲基汞和乙基汞的分析方法.以0.5mol/L 的硝酸溶液为浸提剂,超声波提取1 h,在优化的仪器条件下测定,甲基汞和乙基汞的质量浓度在0.1～50ng/mL 范围内与谱线强度呈良好线性关系（r ≥ 0.999）,检出限分别为0.1,0.2 ng/mL ;加标回收率分别为89.26%～94.26%,76.88%～79.27% ;相对标准偏差分别为1.67%～2.38%,2.58%～3.84%（n=5）.该方法样品前处理简单、重现性好、检出限低、准确度高,适合于农田土壤中甲基汞和乙基汞的同时测定.

A HPLC–ICP/MS method for determination of methyl mercury and ethyl mercury in field soil wasproposed. The methyl mercury and ethyl mercury was separated by using C18 column and detected with ICP–MS. Themethyl mercury and ethyl mercury in field soil were extracted with 0.5 mol/L of nitric acid solution and using theultrasonic assisted extraction. The linear range of the methyl mercury and ethyl mercury were 0.1–50 ng/mL,thecorrelation coefficients were more than 0.999. The detection limits （LOD） of two compounds were 0.1 ng/mL and 0.2ng/mL. The recoveries of the methyl mercury and ethyl mercury were 89.26%–94.26% and 76.88%–79.27%,and therelative standarddeviation（RSD,n=5） were 1.67%–2.38% and 2.58%–3.84%,respectively. The pretreatment of the methodis simple,the reproducibility is good,LOD is low and accuracy is high,so the method is suitable for determination of themethyl mercury and ethyl mercury in field soils.