HPLC-ICP-MS联用技术在富硒金针菇硒的形态分析中的应用

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.

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

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.