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电感耦合等离子体质谱联用技术在元素形态分析中的应用进展

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刘崴, 胡俊栋, 杨红霞, 陈俊良. 电感耦合等离子体质谱联用技术在元素形态分析中的应用进展[J]. 岩矿测试, 2021, 40(3): 327-339. doi: 10.15898/j.cnki.11-2131/td.202006110089
引用本文: 刘崴, 胡俊栋, 杨红霞, 陈俊良. 电感耦合等离子体质谱联用技术在元素形态分析中的应用进展[J]. 岩矿测试, 2021, 40(3): 327-339. doi: 10.15898/j.cnki.11-2131/td.202006110089
shu
LIU Wei, HU Jun-dong, YANG Hong-xia, CHEN Jun-liang. Research Progress on Elemental Speciation Analysis by Inductively Coupled Plasma-Mass Spectrometry Hyphenated Techniques[J]. Rock and Mineral Analysis, 2021, 40(3): 327-339. doi: 10.15898/j.cnki.11-2131/td.202006110089
Citation: LIU Wei, HU Jun-dong, YANG Hong-xia, CHEN Jun-liang. Research Progress on Elemental Speciation Analysis by Inductively Coupled Plasma-Mass Spectrometry Hyphenated Techniques[J]. Rock and Mineral Analysis, 2021, 40(3): 327-339. doi: 10.15898/j.cnki.11-2131/td.202006110089
shu

电感耦合等离子体质谱联用技术在元素形态分析中的应用进展

  • 1.

    国家地质实验测试中心, 中国地质调查局元素微区形态分析重点实验室, 北京 100037

  • 2.

    中国地质调查局, 北京 100037

  • 3.

    中国原子能科学研究院核安全研究所, 北京 102413

  • 基金项目:
    中国地质调查局地质调查项目（DD20190589）；中国地质科学院基本科研业务费项目（CSJ202014）；国家地质实验测试中心大型科研仪器开放共享后补助资金项目（GXBZ-2021-01）
详细信息
    作者简介: 刘崴, 硕士, 副研究员, 主要研究方向为痕量超痕量元素形态分析方法及其应用。E-mail: hattieliu@126.com

  • 中图分类号: O657.63

Research Progress on Elemental Speciation Analysis by Inductively Coupled Plasma-Mass Spectrometry Hyphenated Techniques

  • 1.

    National Research Center for Geoanalysis, Key Laboratory of Element Microareas and Speciation Analysis, China Geological Survey, Beijing 100037, China

  • 2.

    China Geological Survey, Beijing 100037, China

  • 3.

    Institute of Nuclear Safety, China Institute of Atomic Energy, Beijing 102413, China

    摘要

  • 电感耦合等离子体质谱（ICP-MS）作为一种高灵敏度的分析技术在痕量超痕量无机元素分析方面已被广泛应用，其与色谱分离技术相结合为元素形态分析提供了强有力的检测工具。本文阐述了近年来利用不同ICP-MS联用技术进行元素形态分析的研究进展，主要包括：①气相色谱-电感耦合等离子体质谱联用技术（GC-ICP-MS）；②毛细管电泳-电感耦合等离子体质谱联用技术（CE-ICP-MS）；③离子色谱-电感耦合等离子体质谱联用技术（IC-ICP-MS）；④高效液相色谱-电感耦合等离子体质谱联用技术（HPLC-ICP-MS）。在此基础上归纳总结了中国元素形态分析领域的主要研究情况，对元素形态分析发展前景作了展望。这些联用技术中，GC-ICP-MS的灵敏度高，样品传输率接近100%，但其适用于易挥发或中等挥发性样品的分离，应用范围相对较窄；CE-ICP-MS的分离效率高，样品和试剂消耗量少，但受到其进样量限制使得最低检出浓度较大；IC-ICP-MS主要分析阴离子和阳离子及小分子极性化合物，是液相色谱的有益补充，具有分离效果好和快速方便等优点，但离子色谱流动相中的盐类会造成ICP-MS进样管和采样锥的堵塞，使得基体效应严重；HPLC-ICP-MS以其广泛的应用范围、简单的接口技术，成为元素形态分析研究中应用最广泛的联用技术。本文认为，元素形态分析研究中开展复杂基体样品前处理方法研究，研制系列元素形态分析标准物质，建立多元素形态同时分析方法是元素形态分析领域的发展方向。

    BACKGROUND

    As a highly sensitive analytical technique, ICP-MS has been widely used in the analysis of trace inorganic elements. Combined with chromatographic separation technology, it provides a powerful detection tool for elemental speciation analysis.

     OBJECTIVES

    To summarize the research progress of elemental speciation analysis by inductively coupled plasma mass spectrometry hyphenated techniques.

     METHODS

    The main methods of elemental speciation analysis by ICP-MS hyphenated techniques were summarized and compared. The methods included: (1) Gas chromatography coupled with ICP-MS (GC-ICP-MS). (2) Capillary electrophoresis coupled with ICP-MS (CE-ICP-MS). (3) Ion chromatography coupled with ICP-MS (IC-ICP-MS). (4) High performance liquid chromatography coupled with ICP-MS (HPLC-ICP-MS). The main application fields of elemental speciation analysis in China were biomedical field, food and drug safety monitoring and ecoenvironmental geochemistry.

     RESULTS

    GC-ICP-MS has high sensitivity and is suitable for volatile samples, its application is thus limited. CE-ICP-MS has fast analysis and high separation efficiency, but the limitation of sample injection volume makes the method detection limitation high. IC-ICP-MS mainly analyzes anions, cations and small molecular polar compounds. It is a useful complement to HPLC, but the mobile phase containing inorganic salts may block the sampling cone. HPLC-ICP-MS has been the most widely used technology in speciation analysis because of its wide application fields and simple technology.

     CONCLUSIONS

    Sample preparation research for complex matrices, preparing standard materials, and developing simultaneous multi-element speciation analysis methods are the research direction of elemental speciation analysis.
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  • 表 1  砷硒汞铅元素形态分析技术在食品领域的应用研究

    Table 1.  Application of As, Se, Hg and Pb speciation analysis in the food field

    元素 样品 主要色谱条件 分析性能 参考文献
    As 水稻 色谱柱：Hamilton PRP-X100；流动相：20mmol/L磷酸氢二铵和5%甲醇，等度洗脱 可检测As(Ⅲ)、As(Ⅴ)、MMA、DMA、ASA五种砷形态，检出限0.15~0.36μg/L 耿安静等[55]
    鸡肉和鸡肝 色谱柱：Dionex IonPac AS 7；流动相A：3.85mmol/L碳酸铵，流动相B：300mmol/L碳酸铵，梯度洗脱 可检测ROX、ASA、NPAA、CBS、As(Ⅲ)、As(Ⅴ)、MMA、DMA、AsB、AsC十种砷形态，检出限0.3~1.5μg/kg 吴思霖等[56]
    果汁 色谱柱：Prodigy 3 μODS(3)；流动相：5mmol/L丙二酸，3mol/L TBA，5%甲醇，等度洗脱 可检测As(Ⅲ)、DMA、MMA、As(Ⅴ)四种砷形态，检出限0.25、0.33、0.3、0.25μg/L Wang等[57]
    袋泡茶 色谱柱：Dionex IonPac AS19；流动相：30mmol/L碳酸铵，等度洗脱 可检测As(Ⅲ)、As(Ⅴ)、MMA、DMA、AsB五种砷形态，检出限0.04~0.08μg/L 李晓玉等[58]
    植物源保健食品 色谱柱：Thermo SCIENTIFIC AS7；流动相A: 0.35g/L碳酸铵；流动相B: 8g/L碳酸铵，梯度洗脱 可检测As(Ⅲ)、As(Ⅴ)、MMA、DMA、AsB、AsC六种砷形态，检出限0.23~0.54ng/mL 孟珊等[59]
    Se 奶粉 色谱柱：Hamilton PRP-X100；流动相：5mmol/L柠檬酸，10mmol/L乙酸铵，0.1%三氟乙酸，等度洗脱 可检测Se(Ⅳ)、Se(Ⅵ)、SeMet、Se(Cys)2四种硒形态，检出限0.03~0.10μg/L 林立等[60]
    茶叶 色谱柱：Hamilton PRP-X100；流动相A: 10mmol/L柠檬酸，流动相B: 超纯水；梯度洗脱 可检测Se(Ⅳ)、Se(Ⅵ)、SeMet、Se(Cys)2、MeSeCys五种硒形态，检出限0.13~1.09μg/L 陈贵宇等[61]
    苹果 色谱柱：Hamilton PRP-X100；流动相：5mmol/L柠檬酸，等度洗脱 可检测Se(Ⅳ)、Se(Ⅵ)、SeMet、Se(Cys)2、MeSeCys五种硒形态，检出限0.6~1.0μg/L 姚真真等[62]
    小麦 色谱柱：Hamilton PRP-X100；流动相：6mmol/L柠檬酸，等度洗脱 可检测Se(Ⅳ)、Se(Ⅵ)、SeMet、Se(Cys)2四种硒形态，检出限0.15~0.3μg/L 秦冲等[63]
    牛蒡和三七 色谱柱：Hamilton PRP-X100；流动相：8mol/L柠檬酸，等度洗脱 可检测Se(Ⅳ)、Se(Ⅵ)、SeMet、Se(Cys)2四种硒形态，检出限0.033~0.3ng/mL 曹玉嫔等[64]
    Hg 鱼肉 色谱柱：ZORBAX Eclipse Plus C18；流动相A：10mmol/L乙酸铵，0.12%半胱氨酸，流动相B：甲醇，梯度洗脱 可检测Hg(Ⅱ)、MeHg、EtHg三种汞形态，检出限 < 6.2μg/kg 张珂等[65]
    野生菌 色谱柱：Welch Ultimate XB C8；流动相A：甲醇，流动相B：10 mol/L醋酸铵，0.8g/L半胱氨酸，梯度洗脱 可检测Hg(Ⅱ)、MeHg、EtHg、PhHg四种汞形态，检出限0.6~4.5μg/kg Zou等[66]
    海参 色谱柱：Agilent ZORBAX SB-C18；流动相：8%甲醇，92%含0.12%半胱氨酸、0.01 mol/L醋酸铵水溶液，等度洗脱 可检测Hg(Ⅱ)、MeHg、EtHg三种汞形态，检出限分别为0.12、1.6、4.0μg/kg Liu等[67]
    Pb 水产品 色谱柱：Hypersil GLOD C18；流动相：乙二胺四乙酸二钠-乙酸钠溶液+甲醇(75+25，V/V)，等度洗脱 可检测无机铅、三甲基铅、三乙基铅，检出限均为0.01mg/kg 李杰等[68]
    海藻 毛细管柱：未涂层熔融石英毛细管；缓冲溶液：70mmol/L硼酸, 17.5mmol/L硼砂
    (Na2B4O7)    		 可检测无机铅、三甲基铅、三乙基铅，检出限0.091~0.03μg/L 李景喜等[69]
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收稿日期:  2020-06-11
修回日期:  2020-12-21
录用日期:  2021-03-29
刊出日期:  2021-05-28

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