微波消解-电感耦合等离子体质谱法同时测定金华火腿中7种元素

Simultaneous determination of 7 elements in Jinhua hams by microwave digestion and inductively coupled plasma mass spectrometry

目的 建立微波消解-电感耦合等离子体质谱(ICP-MS)同时测定火腿中7种元素(铅、镉、汞、砷、铬、镍、铜)的方法,并用于金华市售火腿中有害元素污染水平的调查。方法 样品经组织捣碎,采用微波消解法预处理,电感耦合等离子体质谱法测定。通过选用钪(Sc)、铑(Rh)、铼(Re)为内标元素,对机体效应、仪器信号漂移进行了补偿,优化仪器的各项参数。结果 方法具有良好的线性关系,相关系数(r)均> 0. 999 0。7种元素的检出限为3. 0μg/kg~4. 0μg/kg,加标回收率为86. 0%~107. 1%,相对标准偏差为4. 9%~11. 8%。检测的100份火腿样品中,7种元素的检出率在3. 0%~100. 0%,总合格率为100%。结论 该法简单、灵敏、准确,能够满足火腿中多元素的快速检测要求。同时,实验结果表明金华市售火腿有害元素污染轻,食用安全性较高。

Objective To establish a method for the determination of 7 elements including Pb,Gd,Hg,As,Cr,Ni and Cu in hams by microwave digestion and inductively coupled plasma mass spectrometry,and to investigate pollution level of deleterious elements in Jinhua market.Methods All samples were mashed,and digested with nitric acid by microwave digestion method and determined by ICP-MS.By using Sc,Rh,Re as the internal standard elements to reduce the matrix interference and the instrument signal drift,the working conditions of instrument were optimized.Results The method had a good linear relationship,and the correlation coefficients(r)were all greater than 0.9990.The detection limits of 7 elements were in the range of 3.0μg/kg-4.0 μg/kg,and the average spiked recoveries were within 86.0%-107.1%,with the relative standard deviation(RSD)ranging of 4.9%-11.8%.The detection rates were between 3.0%-100.0%,and the total qualified rates were 100%.Conclusion The method is easy,quick and accurate,and can meet the requirements for rapid detection of multiple elements in ham.There was no obvious deleterious elements contamination in commercial Jinhua hams.