微波消解-ICP-MS同时测定健腰密骨片中5种重金属及有害元素及其不确定度评定  

Simultaneous Determination and Evaluation of Measurement Uncertainty of Five Heavy Metals and Harmful Elements in Jianyao Migu Tablets by Microwave Digestion-ICP-MS

作　　者：徐婷 陶金 岳镭 XU Ting;TAO Jin;YUE Lei(Test Center of Shanghai Hutchison Pharmaceuticals,Shanghai 201401,China)

机构地区：[1]上海和黄药业有限公司检测中心,上海201401

出　　处：《现代中药研究与实践》2023年第6期58-62,共5页Research and Practice on Chinese Medicines

摘　　要：目的建立微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定健腰密骨片中铜(^(63)Cu)、砷(^(75)As)、镉(^(111)Cd)、汞(^(202)Hg)和铅(^(208)Pb)的含量,并科学评估含量结果不确定度。方法加入硝酸并按设定的程序进行微波消解处理,选取锗(^(72)Ge)、铟(^(115)In)、铋(^(209)Bi)元素作为内标物质,采用ICPMS法同时测定5种重金属及有害元素含量,并参考CNAS-GL006:2019《化学分析中的不确定度评估指南》进行不确定度评估。结果建立的5种重金属及有害元素测定方法线性关系良好,r均大于0.999,重复性RSD均小于8%,加样回收率结果在83.3%~103.4%范围内,计算扩展不确定度后,5种元素测定结果分别为^(63)Cu(0.621±1.89×10^(-2))mg/kg、^(75)As(0.108±1.09×10^(-2))mg/kg、^(111)Cd(0.004±4.68×10^(-4))mg/kg、^(202)Hg(0.045±1.89×10^(-3))mg/kg、^(208)Pb(0.014±8.88×10^(-4))mg/kg,均未超过标准限度。结论建立的方法准确、高效,灵敏度高,并为ICP-MS检测不确定度评估提供依据。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 copper(^(63)Cu),arsenic(^(75)As),cadmium(^(111)Cd),mercury(^(202)Hg)and plumbum(^(208)Pb),and evaluate measurement uncertainty of their content in Jianyao Migu Tablets.Methods Jianyao Migu Tablets were pretreated by nitric acid solution and microwave digestion,germanium(^(72)Ge),indium(^(115)In),and bismuth(^(209)Bi)were selected as internal standard elements for the simultaneous determination of five heavy metals elements by ICP-MS,uncertainty of their content were measured refered to CNAS-GL006:2019 Guidelines for the Evaluation of Uncertainty in Chemical Analysis.Results Five heavy metalselements had good linearity in the selected concentration range,correlation coefficients all reached above 0.999.The repeatability and precision were investigated,RSDs were all below 8%.The recovery rates of each element ranged from 83.3% to 103.4%.Inspection results were(0.621±1.89×10^(-2))mg/kg for ^(63)Cu,(0.108±1.09×10^(-2))mg/kg for 75As,(0.004±4.68×10^(-4))mg/kg for ^(111)Cd,(0.045±1.89×10^(-3))mg/kg for ^(202)Hg and(0.014±8.88×10^(-4))mg/kg for ^(208)Pb with the uncertainty of measurement results evaluated,not exceeding the standard.Conclusion The method has the advantages of rapid analysis,high sensitivity and accuracy,vohich provide a basis for evaluating the uncertainty of ICP-MS detection.

关 键 词：健腰密骨片 电感耦合等离子质谱 重金属及有害元素 微波消解 不确定度 

分 类 号：R284.1[医药卫生—中药学]