微波消解—动态反应池电感耦合等离子体质谱测定农产品中的痕量

doi:10.3969/j.issn.1004-1524.2018.08.20

浙江农业学报 ›› 2018, Vol. 30 ›› Issue (8): 1414-1419.DOI: 10.3969/j.issn.1004-1524.2018.08.20

微波消解—动态反应池电感耦合等离子体质谱测定农产品中的痕量

杏朝刚, 袁京群, 李士敏^*

浙江大学农生环测试中心,浙江杭州310058

收稿日期:2017-11-27 出版日期:2018-08-25 发布日期:2018-08-28
通讯作者: 李士敏,E-mail:shiminli@zju.edu.cn
作者简介:杏朝刚(1987—),男,河北邯郸人,硕士,实验师,主要从事食品及药品安全检测方法研究。E-mail:xcg@zju.edu.cn
基金资助:
原农业部食用农产品风险评估专项(GJFP2017015)

Determination of trace selenium in agricultural products with microwave digestion-dynamic reaction cell inductively coupled plasma mass spectrometry

XING Chaogang, YUAN Jingqun, LI Shimin^*

Analysis Center of Agrobiology and Environmental Sciences of Zhejiang University, Hangzhou 310058, China

Received:2017-11-27 Online:2018-08-25 Published:2018-08-28

摘要/Abstract

摘要： 建立用微波消解-动态反应池电感耦合等离子体质谱测定农产品中痕量硒的方法:HNO₃经密闭微波消解系统处理农产品样品,以CH₄为反应气,采用动态反应池(DRC)技术消除m/z 80处⁴⁰Ar⁴⁰Ar⁺对硒测定的干扰。系统考查反应气种类、流速、抑制参数q(RPq)等对信噪比(S/B)的影响。实验结果表明,当以⁸⁰Se为分析物、CH₄为反应气、流速为0.9 mL·min^-1、RPq=0.7时可以有效消除干扰,信噪比最佳。该方法的线性范围为0.01~200 μg·L^-1,检出限为0.001 μg·g^-1,定量限为0.004 μg·g^-1,7次平行测定值的相对标准偏差(RSD) 为3.39%,加标回收率为97.32%~101.1%。采用该方法对国家标准柑橘叶参考物质GBW10020进行分析,测定结果和标准值吻合。

关键词: 仪器分析, 元素检测, 硒

Abstract: A dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) method was proposed for the determination of trace selenium in agricultural products digested in closed vessel microwave with nitric acid. Application of methane as the reactive cell gas in the DRC reduced the argon dimer interferences at selenium masses m/z 80. The effects of the reaction gas species, flow rate and rejection parameter q (RPq) of the DRC system on signal-to-background ratio were studied. It was shown that the interference was eliminated when CH₄ was used as reaction gas with flow rate of 0.9 mL·min^-1, and RPq was 0.7. The proposed method had a wide linear range of 0.01~200 μg·L^-1 and a low limit of detection and quantitation (0.001 μg·g^-1 and 0.004 μg·g^-1, respectively). The relative standard deviation was 3.39% (n=7), and the recoveries were between 97.32%~101.1%. Validation of the method was carried out by determining Se in standard reference citrus leaves GBW10020. Good agreement was obtained between the certified value and the experimental result.

Key words: instrumental analysis, element determination, selenium

中图分类号:

O657.63
S13

杏朝刚, 袁京群, 李士敏. 微波消解—动态反应池电感耦合等离子体质谱测定农产品中的痕量[J]. 浙江农业学报, 2018, 30(8): 1414-1419.

XING Chaogang, YUAN Jingqun, LI Shimin. Determination of trace selenium in agricultural products with microwave digestion-dynamic reaction cell inductively coupled plasma mass spectrometry[J]. , 2018, 30(8): 1414-1419.

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微波消解—动态反应池电感耦合等离子体质谱测定农产品中的痕量

Determination of trace selenium in agricultural products with microwave digestion-dynamic reaction cell inductively coupled plasma mass spectrometry

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