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微波消解-电感耦合等离子体质谱法测定生物样品中微量硒的方法研究

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文章导航 > 岩矿测试 > 2014 > 33(1): 34-39

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冯永明, 邢应香, 刘洪青, 章勇. 微波消解-电感耦合等离子体质谱法测定生物样品中微量硒的方法研究[J]. 岩矿测试, 2014, 33(1): 34-39.
引用本文: 冯永明, 邢应香, 刘洪青, 章勇. 微波消解-电感耦合等离子体质谱法测定生物样品中微量硒的方法研究[J]. 岩矿测试, 2014, 33(1): 34-39.
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Yong-ming FENG, Ying-xiang XING, Hong-qing LIU, Yong ZHANG. Determination of Trace Selenium in Biological Samples by Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion[J]. Rock and Mineral Analysis, 2014, 33(1): 34-39.
Citation: Yong-ming FENG, Ying-xiang XING, Hong-qing LIU, Yong ZHANG. Determination of Trace Selenium in Biological Samples by Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion[J]. Rock and Mineral Analysis, 2014, 33(1): 34-39.
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微波消解-电感耦合等离子体质谱法测定生物样品中微量硒的方法研究

  • 1.

    安徽省地质实验研究所， 安徽 合肥 230001

  • 2.

    赛默飞世尔科技(上海)有限公司， 上海 201206

详细信息
    作者简介: 冯永明，工程师，精细化工专业。E-mail: fengyongm@sina.com
    通讯作者: 邢应香，助理工程师，化学专业.E-mail:yingxiangxing@163.com

  • 中图分类号: O613.52; O657.31; O657.63

Determination of Trace Selenium in Biological Samples by Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion

  • 1.

    Anhui Research Institute of Geological Experiment, Hefei 230001, China

  • 2.

    ThermoFisher Scientific (Shanghai) Corporation, Shanghai 201206， China

More Information

    摘要
  • 生物样品中微量元素硒的分析检测，经典方法是湿法消解-氢化物发生原子荧光光谱法(HG-AFS)。湿法消解处理生物样品需使用大量试剂，并且消解时间长，样品背景值高；HG-AFS的分辨率较低，已经不能满足微量硒的分析需求。解决生物样品的消解过程缓慢、试剂用量大的问题是提高样品中微量元素硒的检出限和分辨率的前提。本文采用湿法消解和微波消解两种消解体系处理样品，对两种方法制备的溶液分别采用HG-AFS和电感耦合等离子体质谱法(ICP-MS)进行测定，通过对比试验确定了微波消解ICP-MS方法可以实现生物样品中微量硒的准确测定。对比试验表明：采用高压密闭微波消解前处理样品技术可以大大缩短消解时间，减少试剂用量，降低了样品背景值；利用ICP-MS直接进行测定，方法检出限为0.01 μg/g，精密度(RSD，n=12)小于4%，低于HG-AFS的检出限(0.03 μg/g)和精密度(<10%)。微波消解ICP-MS方法操作简单快捷，降低了方法检出限，提高了样品分析的准确度和精密度。
    Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS) with wet digestion is classical method to determine the trace element selenium in biological samples. The analytical requirements cannot be met by low resolution HG-AFS and wet digestion processing and carries the additional disadvantages of high quantities of reagent consumption, lengthy processing time and production of high background values. Accelerating digestion processing time and reducing the amount of reagent consumption have been considered as prerequisites for increasing detection limit and resolution of selenium. In this article, samples were analyzed by HG-AFS and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) after two different sample pretreatments of wet digestion and microwave digestion. The method of ICP-MS with microwave digestion was established through these contrast tests. The results indicate that microwave digestion can reduce digestion time, decrease reagent consumption and lower background in high-pressure sealed conditions. Detection limits of HG-AFS and ICP-MS are 0.03 μg/g and 0.01 μg/g, respectively. In addition, according to the determination for national standard reference samples, relative standard deviations of HG-AFS and ICP-MS are less than 10% and 4%, respectively. Obviously, low detection limits and improved accuracy and precision can been acquired by direct analysis with ICP-MS. The established method is simple to operate and can been conducted for the rapid determination of trace selenium in various biological samples.
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  • 表 1  ICP-MS仪器工作条件

    Table 1.  Working parameters of the ICP-MS instrument

    工作参数设定条件工作参数设定条件
    功率1350 W测量方式跳峰
    冷却气(Ar)流量13.0 L/min扫描次数50
    辅助气(Ar)流量0.7 L/min停留时间/通道10 ms
    雾化气(Ar)流量0.8 L/min每个质量通道数3
    采样锥(Ni)孔径1.0 mm总采集时间20 s
    截取锥(Ni)孔径0.7 mm固定工作频率27.12 MHz
    下载: 导出CSV

    表 2  微波消解程序

    Table 2.  Procedure of the microwave digestion

    步骤消解时间t/min消解功率P/W 消解温度θ/℃
    151000140
    2101000190
    3151000200
    420--
    下载: 导出CSV

    表 3  HG-AFS测定两种消解方法制备溶液中的硒

    Table 3.  Analytical results of Se in solutions prepared with two pretreatment methods by HG-AFS

    标准物质编号w(Se)/(μg·g-1)
    湿法消解样品测定值微波消解样品测定值标准值
    GBW 100100.0550.0580.062
    GBW 100110.0490.0490.053
    GBW 100120.0150.0180.021
    GBW 100140.1780.1860.200
    GBW 100150.0800.0870.092
    GBW 100160.0850.0920.098
    下载: 导出CSV

    表 4  HG-AFS测定微波消解和湿法消解的样品空白值

    Table 4.  The blank values of Se in solutions prepared with two pretreatment methods by HG-AFS

    样品编号w(Se)/(μg·g-1)
    湿法消解样品测定值微波消解样品测定值
    BL10.01270.0011
    BL20.01080.0012
    BL30.00960.0014
    BL40.01160.0012
    BL50.00970.0017
    BL60.00920.0010
    BL70.00910.0015
    BL80.01090.0010
    BL90.01160.0018
    BL100.01000.0014
    BL110.01100.0016
    BL120.01230.0015
    下载: 导出CSV

    表 5  ICP-MS测定两种消解方法制备溶液中的硒

    Table 5.  Analytical results of Se in solutions prepared with two pretreatment methods by ICP-MS

    标准物质编号w(Se)/(μg·g-1)
    湿法消解样品测定值微波消解样品测定值标准值
    GBW 100100.0670.0600.062
    GBW 100110.0590.0520.053
    GBW 100120.0250.0190.021
    GBW 100140.2320.1920.200
    GBW 100150.0990.0890.092
    GBW 100160.1050.0930.098
    下载: 导出CSV

    表 6  ICP-MS测定微波消解和湿法消解的样品空白值

    Table 6.  The blank values of Se in solutions prepared with two pretreatment methods by ICP-MS

    样品编号w(Se)/(μg·g-1)
    湿法消解样品测定值微波消解样品测定值
    BL10.01070.0009
    BL20.01080.0009
    BL30.00960.0009
    BL40.01160.0012
    BL50.00970.0011
    BL60.00920.0009
    BL70.00910.0012
    BL80.01090.0010
    BL90.01160.0013
    BL100.01120.0010
    BL110.01200.0010
    BL120.01230.0014
    下载: 导出CSV

    表 7  标准物质的测定结果

    Table 7.  Analytical results of Se in the standard materials

    标准物质编号w(Se)/(μg·g-1) 相对偏差/%RSD/%
    平均测定值标准值
    GBW 100100.0650.062 0.261.1
    GBW 100110.0570.053-0.241.2
    GBW 100120.0190.021 0.292.4
    GBW 100140.2130.200 0.162.4
    GBW 100150.0870.092-0.483.1
    GBW 100160.1010.0980 0.181.0
    下载: 导出CSV

    表 8  实际样品的分析结果

    Table 8.  Analytical results of Se in real samples

    实际样品w(Se)/(μg·g-1) 实际样品w(Se)/(μg·g-1)
    水稻籽实10.035 脱水蔬菜20.256
    水稻籽实20.046脱水蔬菜30.241
    水稻籽实30.058茶叶10.085
    水稻籽实40.064茶叶20.074
    脱水蔬菜10.187茶叶30.068
    下载: 导出CSV
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收稿日期:  2013-07-01
录用日期:  2013-09-17

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