微波消解-ICP-MS同时测定安息香中5种重金属及有害元素

Simultaneous Determination of Five Heavy Metals and Harmful Elements in Benzoinum by Microwave Digestion-ICP-MS

目的:建立微波消解-电感耦合等离子体质谱法(ICP-MS)测定安息香中铅(Pb)、镉(Cd)、砷(As)、汞(Hg)和铜(Cu)的含量,并分析我国4个药材市场所售安息香药材含重金属及有害元素情况。方法:安息香药材加入硝酸-过氧化氢溶液,采用微波消解法进行前处理,选取锗(Ge)、铟(In)、铋(Bi)元素作为内标,采用ICP-MS同时测定Pb、Cd、As、Hg和Cu 5种重金属及有害元素含量。结果:5种元素在所选质量浓度范围内具有良好的线性关系,相关系数≥0.9996。各元素回收率为80.89%~102.70%,检出限为0.0018~0.0173 mg·kg^(–1)。对重复性、精密度进行考察,相对标准偏差(RSD)均小于5.0%。测定32批安息香药材中5种重金属及有害元素平均含量顺序为Pb>Cu>Hg>As>Cd,其中Hg的检出率为100%。结论:该方法操作简单、分析快速、灵敏度和准确度高,可检测安息香药材中重金属及有害元素的含量,适用于安息香药材的质量控制。

Objective:To establish a method based on microwave digestion-inductively coupled plasma-mass spectrometry(ICP-MS)to determine the content of five heavy metals and harmful elements,including plumbum(Pb),cadmium(Cd),arsenic(As),mercury(Hg),and copper(Cu)and analyze the current situation of their content in Benzoinum sold in four major herbal markets in China.Methods:Benzoinum were pretreated by nitric acid-hydrogen peroxide solution and microwave digestion,and germanium(Ge),indium(In),and bismuth(Bi)were selected as internal standard elements for the simultaneous determination of Pb,Cd,As,Hg,and Cu by ICP-MS.Results:The five heavy metal elements had good linearity in the selected concentration range,and the correlation coefficients all reached above 0.9996.The recovery rates of each element ranged from 80.89%to 102.70%,and the detection limits were 0.0018-0.0173 mg·kg^(–1).The repeatability and precision were investigated,and the relative standard deviations(RSDs)were all below 5.0%.Using this method to determine 32 batches of Benzoinum,the order of average content of five common heavy metals and harmful elements was Pb>Cu>Hg>As>Cd,and the detection rate of Hg was 100%.Conclusion:The method has the advantages of simple operation,rapid analysis,and high sensitivity and accuracy,which can monitor the content of heavy metals and harmful elements in Benzoinum and is suitable for the quality control of Benzoinum.