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HPLC-ICP-MS联用技术在富硒金针菇硒的形态分析中的应用

铁梅1, 方禹之2, 孙铁彪1, 李闯1, 费金岩1, 李华为3, 臧树良1   

    1. 辽宁大学环境科学系, 沈阳 110036;
    2. 华东师范大学化学系, 上海 200062;
    3. 沈阳师范大学化学与生命科学学院, 沈阳 110034
  • 收稿日期:2006-08-06 修回日期:1900-01-01 出版日期:2007-04-10 发布日期:2007-04-10
  • 通讯作者: 臧树良

Application of HPLC-ICP-MS in Speciation Analysis of Selenium in Selenized Flammulina velutipes

TIE Mei1, FANG Yu-Zhi2, SUN Tie-Biao1, LI Chuang1, FEI Jin-Yan1, LI Hua-Wei3, ZANG Shu-Liang1*   

    1. Department of Environmental Science, Liaoning University, Shenyang 110036, China;
    2. Department of Chemistry, East China Normal University, Shanghai 200062, China;
    3. College of Environmental and Life Sciences, Shenyang Normal University, Shenyang 110034, China
  • Received:2006-08-06 Revised:1900-01-01 Online:2007-04-10 Published:2007-04-10
  • Contact: ZANG Shu-Liang

摘要: 从富硒培养的金针菇中分离得到含硒化合物, 并采用SE-HPLC-ICP-MS联机技术对浸提液中的含硒化合物进行分离分析; 同时对样品中的硒蛋白在特定条件下水解, 采用RP-HPLC-ICP-MS联机技术对水解液中硒代氨基酸进行确认, 并测定其中硒的含量. 结果表明, 可溶态硒是富硒金针菇中硒的主要存在形式, 其中小分子含硒有机化合物中的含硒量占浸提液中硒的71.87%; 而含硒蛋白所占比例为4.88%; 进一步确定富硒金针菇中含有硒代胱氨酸、硒代蛋氨酸和由二者组成的含硒多肽等, 各形态硒的含量为总硒量的12.3%, 17.6%和36.8%. 本方法将具有高效分离能力的色谱技术与高灵敏度的元素检测技术成功结合, 用于含硒生物分子中硒的在线分析, 具有快速、灵敏及准确等特点.

关键词: 金针菇, 形态分析, 硒, HPLC-ICP-MS

Abstract: The determination of selenium in different selenium-containing compounds extracted from selenized Flammulina velutipes was studied by SEC-DADICP-MS-ICP-MS. After hydrolyzation of the different compounds under special condition, selenium-amino acid in the leaching solution was confirmed by RPLC-DADICP-MS-ICP-MS. A new selenium-containing compound was detected and the content of selenium in differnt offspring by hydrolyzation was determined. It is shown that the soluble selenium was the main existing form in selenized Flammulina velutipes, and the content of selenium in compounds low molecular weight accounting for 71.87% of the total amount was much higher than that in compounds with a high molecular weight. Then the further results show that in selenized Flammulina velutipes there mainly are Se-Cys, Se-Met, peptide composed by the former two. The max content of selenium in the three main speciations accounted for 12.3%, 17.6%, 36.8%. This method combined by HPLC and better sensitive element detect technology can be successfully applied in the online determination of selenium in selenium-containing biological molecule.

Key words: Flammulina velutipes, Speciation analysis, Selenium, HPLC-ICP-MS

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