稀氨水-微波消解-电感耦合等离子体质谱法测定生态地球化学生物样品中的碘  

Determination of iodine in biological samples of ecosystem geochemistry by inductively coupled plasma mass spectrometry with dilute ammonia water and microwave digestion

作　　者：刘伟 沈桂华 黄瑜 彭天赐 张文娟 LIU Wei;SHEN Guihua;HUANG Yu;PENG Tianci;ZHANG Wenjuan(Geological and Mineral Testing Research Center of Guangxi Zhuang Autonomous Region,Nanning 530023,Guangxi,China)

机构地区：[1]广西壮族自治区地质矿产测试研究中心,广西南宁530023

出　　处：《矿产与地质》2020年第2期386-390,共5页Mineral Resources and Geology

基　　金：广西科技厅2019年度广西重点研发计划项目“广西贵港富硒水田安全利用集成技术研究与应用示范”(项目编号:2018AB36031,合同编号:桂科AB19245050)资助。

摘　　要：研究建立了稀氨水-微波消解-电感耦合等离子体质谱法(ICP-MS)测定生态地球化学生物样品中碘的方法。通过采用稀氨水代替硝酸对样品进行消解,较好地解决了测定结果不稳定及记忆效应严重现象;同时,采用离线内标加入法,有效地消除了检测过程中因操作因素等引起的误差和基体效应干扰。进行条件优化实验后,该方法的检出限为0.005μg/g,测定范围0.05~12.5μg/g。使用国家一级生物成分分析标准物质验证,相对误差(RE)为0.53%~7.17%,相对标准偏差(RSD)(n=8)为0.87%~5.81%。实际样品测定加标回收率在94.0%~96.7%之间。建立的方法能有效满足生态地球化学生物样品中碘的测试需求。In this paper,a method for the determination of iodine in biological samples of ecosystem geochemistry by inductively coupled plasma mass spectrometry(ICP-MS)with dilute ammonia and microwave digestion has been established.Diluted ammonia is used instead of nitric acid to digest the sample,which solves the unstable determination result and the serious memory effect.At the same time,the off-line internal standard addition method can effectively eliminate the errors and matrix effect interference caused by operation factors in the detection process.After the condition optimization experiment,the detection limit of the method is 0.005μg/g,and the determination range is 0.05–12.5μg/g.Accuracy and precision of the method are tested by analyzing a variety of certified reference materials for the chemical composition of biological samples.The relative error is between 0.53%–7.17%,and the relative standard deviation is between 0.87%–5.81%.The real samples are subjected to a standard recovery test,and the standard recovery rate is between 94.0%and 96.7%.The established method can effectively meet the needs of the determination of iodine in biological samples of ecosystem geochemistry.

关 键 词：碘 稀氨水 生物样品 微波消解 电感耦合等离子体质谱法(ICP-MS) 

分 类 号：O657.63[理学—分析化学] O613.44[理学—化学]