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高效液相色谱-电感耦合等离子体质谱测定大米粉中的硒形态

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邵鹏威, 路国慧, 郑宇, 胡俊栋, 赵全升, 杨永亮, 刘崴. 高效液相色谱-电感耦合等离子体质谱测定大米粉中的硒形态[J]. 环境化学, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
引用本文: 邵鹏威, 路国慧, 郑宇, 胡俊栋, 赵全升, 杨永亮, 刘崴. 高效液相色谱-电感耦合等离子体质谱测定大米粉中的硒形态[J]. 环境化学, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
shu
SHAO Pengwei, LU Guohui, ZHENG Yu, HU Jundong, ZHAO Quansheng, YANG Yongliang, LIU Wei. Determination of selenium species in rice flour using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. Environmental Chemistry, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
Citation: SHAO Pengwei, LU Guohui, ZHENG Yu, HU Jundong, ZHAO Quansheng, YANG Yongliang, LIU Wei. Determination of selenium species in rice flour using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. Environmental Chemistry, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
shu

高效液相色谱-电感耦合等离子体质谱测定大米粉中的硒形态

  • 1. 青岛大学环境科学与工程学院, 青岛, 266071;

  • 2. 国家地质实验测试中心, 北京, 100037

    • 通讯作者: 刘崴, E-mail: hattieliu@126.com
  • 基金项目:

    中国地质科学院基本科研业务费项目（YYWF201620）和中国地质大调查项目（DD20190589）资助.

Determination of selenium species in rice flour using high performance liquid chromatography-inductively coupled plasma mass spectrometry

  • 1. College of Environmental Sciences and Engineering, Qingdao University, Qingdao, 266071, China;

  • 2. National Research Center for Geo-Analysis(NRCGA), Beijing, 100037, China

    • Corresponding author: LIU Wei, hattieliu@126.com
  • Fund Project: Supported by the Research Fund of Chinese Academy of Geological Sciences (YYWF201620) and the Geological Survey Project of China (DD20190589).

  • 摘要: 建立了高效液相色谱-电感耦合等离子体质谱联用技术（HPLC-ICP-MS）测定大米粉中硒代胱氨酸（SeCys2）、甲基-硒代半胱氨酸（MeSeCys）、亚硒酸根（Se（Ⅳ））、硒代蛋氨酸（SeMet）、硒酸根（Se（Ⅵ））等5种硒形态的分析方法.采用Hamilton PRP-X100分析柱，以pH 4和pH 6的20 mmol·L-1的柠檬酸溶液辅以少量甲醇为流动相，在梯度洗脱条件下，9 min内可实现5种硒形态完全分离.SeCys2、MeSeCys、Se（Ⅳ）、SeMet、Se（Ⅵ）的检出限分别为0.88、0.69、1.00、0.90、0.82 μg·L-1.利用富硒小麦粉标准物质RM8436探讨了不同提取方式的提取效果.最终确定75 mmol·L-1 Tris-HCl（pH 7.5）添加XIV蛋白酶和Driselase酶作为提取剂，在37℃振荡提取3 h为大米样品前处理方法.利用该方法分析了富硒地区大米粉中的硒形态，结果表明，大米粉中的硒主要以有机硒形态为主，其中SeMet是最主要的硒形态，占总硒的90%左右.
    Abstract: An analytical method for the determination of five selenium species in rice flour samples was developed using high performance liquid chromatography combined with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Seleno-Cystine(SeCys2), (Methyl)Seleno-Cysteine (MeSeCys), Selenite(Se(Ⅳ)), Selenoate(Se(Ⅵ)) and Selenomethionine (SeMet) were completely separated on a Hamilton PRP-X100 anion exchange column using 20 mmol·L-1 citric acid solution (pH 4.0), 20 mmol·L-1 citric acid solution (pH 6.0) and methyl alcohol as the mobile phase under gradient elution within 9 minutes. The detection limits of SeCys2, MeSeCys, Se(Ⅳ), SeMet and Se(Ⅵ) were 0.88, 0.69, 1.00, 0.90, 0.82 μg·L-1, respectively. 75 mmol·L-1 Tris-HCl (pH 7.5) with XIV protease and Driselase was eventually selected as extractant. Different sample preparation methods had been compared and oscillation method with 3 h at 37 ℃ was chosen finally. This method was applied to measure selenium species in rice flour samples from selenium-enriched areas. The results indicated that SeMet was the main species in rice flour, accounting for about 90% of the total amount of selenium.
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  • 收稿日期:  2019-08-15
邵鹏威, 路国慧, 郑宇, 胡俊栋, 赵全升, 杨永亮, 刘崴. 高效液相色谱-电感耦合等离子体质谱测定大米粉中的硒形态[J]. 环境化学, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
引用本文: 邵鹏威, 路国慧, 郑宇, 胡俊栋, 赵全升, 杨永亮, 刘崴. 高效液相色谱-电感耦合等离子体质谱测定大米粉中的硒形态[J]. 环境化学, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
shu
SHAO Pengwei, LU Guohui, ZHENG Yu, HU Jundong, ZHAO Quansheng, YANG Yongliang, LIU Wei. Determination of selenium species in rice flour using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. Environmental Chemistry, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
Citation: SHAO Pengwei, LU Guohui, ZHENG Yu, HU Jundong, ZHAO Quansheng, YANG Yongliang, LIU Wei. Determination of selenium species in rice flour using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. Environmental Chemistry, 2020, (5): 1434-1441. doi: 10.7524/j.issn.0254-6108.2019081504
shu

高效液相色谱-电感耦合等离子体质谱测定大米粉中的硒形态

    通讯作者: 刘崴, E-mail: hattieliu@126.com
  • 1. 青岛大学环境科学与工程学院, 青岛, 266071;
  • 2. 国家地质实验测试中心, 北京, 100037
  • 收稿日期:  2019-08-15
基金项目:

中国地质科学院基本科研业务费项目（YYWF201620）和中国地质大调查项目（DD20190589）资助.

摘要: 建立了高效液相色谱-电感耦合等离子体质谱联用技术（HPLC-ICP-MS）测定大米粉中硒代胱氨酸（SeCys2）、甲基-硒代半胱氨酸（MeSeCys）、亚硒酸根（Se（Ⅳ））、硒代蛋氨酸（SeMet）、硒酸根（Se（Ⅵ））等5种硒形态的分析方法.采用Hamilton PRP-X100分析柱，以pH 4和pH 6的20 mmol·L-1的柠檬酸溶液辅以少量甲醇为流动相，在梯度洗脱条件下，9 min内可实现5种硒形态完全分离.SeCys2、MeSeCys、Se（Ⅳ）、SeMet、Se（Ⅵ）的检出限分别为0.88、0.69、1.00、0.90、0.82 μg·L-1.利用富硒小麦粉标准物质RM8436探讨了不同提取方式的提取效果.最终确定75 mmol·L-1 Tris-HCl（pH 7.5）添加XIV蛋白酶和Driselase酶作为提取剂，在37℃振荡提取3 h为大米样品前处理方法.利用该方法分析了富硒地区大米粉中的硒形态，结果表明，大米粉中的硒主要以有机硒形态为主，其中SeMet是最主要的硒形态，占总硒的90%左右.

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