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高效液相色谱与电感耦合等离子体质谱联用技术用于胁迫富硒海带硒形态研究

仲娜1,2, 王小如3, 杨黄浩3, 曹煊1, 王庚4   

    1. 中国海洋大学化学化工学院, 青岛 266003;
    2. 青岛市药品检验所, 青岛 266071;
    3. 国家海洋局第一海洋研究所, 青岛现代分析及中药标准化重点实验室, 青岛 266061;
    4. 山东大学化学与化工学院, 济南 250100
  • 收稿日期:2007-04-20 修回日期:1900-01-01 出版日期:2008-01-10 发布日期:2008-01-10
  • 通讯作者: 王小如

Selenium Speciation in Enriched Laminaria Japonica by HPLC-ICP-MS

ZHONG Na1,2, WANG Xiao-Ru3*, YANG Huang-Hao3, CAO Xuan1, WANG Geng4   

    1. College of Chemistry and Chemical Engineering, Ocean University of Qingdao, Qingdao 266003, China;
    2. Qingdao Institute for Drug Control, Qingdao 266071, China;
    3. Key Labortory of Modern Analytical Technology & Standardization of Chinese Medicine of Qingdao, First Institute of Oceanography, State Oceanic Adiministration, Qingdao 266061, China;
    4. College of Chemistry, Shandong University, Jinan 250100, China
  • Received:2007-04-20 Revised:1900-01-01 Online:2008-01-10 Published:2008-01-10
  • Contact: WANG Xiao-Ru

摘要: 通过对海带胁迫富硒培养, 研究了海带对硒的富集总量及硒化学形态转变. 建立了反相离子对缓冲盐等3个色谱系统的高效液相色谱与电感耦合等离子体质谱联用(RP-HPLC-ICP-MS)技术测定亚硒酸钠、硒甲基半胱氨酸(MeSeCys)、硒代蛋氨酸(SeMet)三种硒形态. 采用3种提取溶剂, 超声提取缩短提取时间, 分离检测富硒海带的主要硒形态为亚硒酸钠、硒甲基半胱氨酸和硒代蛋氨酸.

关键词: 富硒海带, RP-HPLC-ICP-MS, SEC-HPLC-ICP-MS, 总量, 形态, 亚硒酸钠, 硒甲基半胱氨酸, 硒代蛋氨酸

Abstract: In the present study, the concentration and speciation of selenium in Laminaria, enriched with selenite during its growth, was performed by establishing a RP-HPLC-ICP-MS method to separate selenite, MeSeCys and SeMet successively. There were three of systems ion-pairing agent and buffer chromatograph: (1) Alltima C8 column, mobile phase: 5 mmol/L citric, 5 mmol/L hexanesulfonic acid(pH 3.5)-methonol(95∶5, volume ratio); (2) Alltima C8 column, mobile phase: water-methnol(98∶2, volume ratio)-0.1%TFA; (3) Alltima C18 column, mobile phase: 20 mmol/L ammonium acetic-methonol(95∶5, volume ratio).Three solvent of 0.1 mol/L HCl, 20 mmol/L Tris-HCl and 20 mmol/L ammonium acetic buffer were used for the extraction of seleno-compound from enriched Laminaria, the major selenospecies determined were selenite, MeSeCys, SeMet, compared with the relative retention time of Se standards.

Key words: Enriched Laminaria, RP-HPLC-ICP-MS, SEC-HPLC-ICP-MS, Total concentration, Speciation, Na2SeO3, MeSeCys, SeMet

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