快速消解-电感耦合等离子体质谱法测定西洋参中15种金属元素的含量  

Determination of 15 Metal Elements in American Ginseng by Inductively Coupled Plasma Mass Spectrometry with Rapid Digestion

作　　者：陈亮 CHEN Liang(Fujian Institute for Food and Drug Quality Control,Fuzhou 350000,China)

机构地区：[1]福建省食品药品质量检验研究院,福州350000

出　　处：《理化检验(化学分册)》2025年第1期22-27,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：福建省药品监督管理局科技项目(2022009)。

摘　　要：提出了快速消解-电感耦合等离子体质谱法(ICP-MS)测定西洋参中15种金属元素(铍、硼、锰、铜、锌、砷、硒、锶、钼、镉、锡、锑、钡、汞、铅)含量的方法。取粉碎并过筛后的西洋参样品0.2 g置于50 mL离心管中,加入2 mL 30%(质量分数)过氧化氢溶液、5 mL硝酸,密封过夜,置于110℃石墨消解仪中消解60 min,冷却至25℃,加入1 mg·L^(-1)金标准使用液200μL,用水定容至50 mL,混匀后离心10 min,上清液用0.45μm水相滤膜过滤,采用ICP-MS测定滤液中上述15种金属元素的含量,在线加入含20μg·L^(-1)钪、锗、铟、铋的内标溶液。结果表明,15种金属元素的质量浓度在一定范围内与对应的内标校正后的信号强度呈线性关系,检出限(3s)为0.002~0.282 mg·kg^(-1);方法用于分析标准物质,15种金属元素的测定值均在认定值的不确定度范围内;按照标准加入法进行回收试验,回收率为89.1%~103%,测定值的相对标准偏差(n=6)均小于6.0%;采用快速消解法和微波消解法消解西洋参样品,各金属元素的测定值基本一致。A method for determination of 15 metal elements,including beryllium,boron,manganese,copper,zinc,arsenic,selenium,strontium,molybdenum,cadmium,tin,antimony,barium,mercury,and lead in American ginseng by inductively coupled plasma mass spectrometry(ICP-MS)with rapid digestion was proposed.0.2 g of crushed and sieved American ginseng sample was taken and placed in a 50 mL-centrifuge tube.2 mL of 30%(mass fraction)hydrogen peroxide solution and 5 mL of nitric acid were added and the mixture was sealed overnight.Then the mixture was placed in a graphite digestion apparatus at 110℃for 60 min and cooled to 25℃.200μL of 1 mg·L^(-1)gold standard solution was added,and the solution was made its volume up to 50 mL with water and mixed well.The solution was centrifuged for 10 min,and the supernatant solution was passed through a 0.45μm water phase filter membrane.15 metal elements in the filtrate were determined by ICP-MS,and 20μg·L^(-1)internal solution,including scandium,germanium,indium,and bismuth,was added online.As shown by the results,linear relationships between the ratios of the corresponding signal intensities after internal standard correction and mass concentrations of 15 metal elements were found in definite ranges,with detection limits(3s)in the range of 0.002-0.282 mg·kg^(-1).This method was used to analyze the standard substance,and the determined values of 15 metal elements were found within the uncertainty range of the certified values.Test for recovery was made by the standard addition method,giving results in the range of 89.1%-103%,with RSDs(n=6)of the determined values less than 6.0%.The rapid digestion method and microwave digestion method were used to digest the American ginseng samples,and the determined values of various metal elements were basically consistent.

关 键 词：快速消解 电感耦合等离子体质谱法(ICP-MS) 西洋参 金属元素 

分 类 号：O657.63[理学—分析化学]