微波消解-ICP/MS法同时测定鱼肉中的砷和汞

Simultaneous Determination of As and Hg in Fish by Microwave Digestion-ICP/MS

采用微波消解处理鱼肉样品,用电感耦合等离子体质谱法测定样品中砷和汞。通过试验优化微波消解参数、酸体系及赶酸温度,用在线加入内标方法消除基体干扰及仪器漂移对测定的影响。方法在0μg/L～40. 0μg/L范围内线性良好,砷和汞的方法检出限分别为0. 002 mg/kg和0. 001 mg/kg,实际样品6次测定结果的RSD为5. 4%～15. 6%,加标回收率为90. 0%～110%。将该方法用于测定芹菜和扇贝标准物质,测定值在标准值不确定度范围内。

The fish samples were treated by microwave digestion,and ICP/MS was used to simultaneously determine arsenic(As)and mercury(Hg).The microwave digestion parameters,acid system and removal tem-perature were optimized,and the internal standards were added online to eliminate the impacts of matrix interfer-ences and instrument drift.The method had good linearity in the range of0μg/L^40.0μg/L,and the detec-tion limits of As and Hg were0.002mg/kg and0.001mg/kg,respectively.The relative standard deviation of actual samples were5.4%~15.6%(n=6),and the recoveries were90.0%~110%.Two certified reference materials were analyzed meanwhile and the results were within the uncertainty of the standard values.