色谱

色谱 ›› 2015, Vol. 33 ›› Issue (3): 215-220.DOI: 10.3724/SP.J.1123.2014.12002

• 研究论文 • 上一篇    下一篇

谷胱甘肽修饰的SiO2@Au核壳填料的制备及其作为毛细管液相色谱和加压电色谱固定相的性能评价

汪慧, 薛芸, 鲁阳芳, 谷雪, 王彦, 阎超   

  1. 上海交通大学药学院, 上海 200240
  • 收稿日期:2014-12-01 修回日期:2015-01-04 出版日期:2015-03-08 发布日期:2015-02-12
  • 通讯作者: 阎超, 王彦
  • 基金资助:

    国家自然科学基金项目(21175092,21105064);国家重大科学仪器设备开发专项(2011YQ150072,2011YQ15007204,2011YQ15007207,2011YQ15007210);上海市自然科学基金项目(12ZR1413600).

Preparation and evaluation of glutathione modified SiO2@Au as stationary phase in capillary liquid chromatography and pressurized capillary electrochromatography

WANG Hui, XUE Yun, LU Yangfang, GU Xue, WANG Yan, YAN Chao   

  1. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China
  • Received:2014-12-01 Revised:2015-01-04 Online:2015-03-08 Published:2015-02-12

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摘要：

利用醛基和氨基之间的席夫碱反应在SiO2微球表面引入聚合物分子聚乙烯亚胺(polyethyleneimine, PEI),以提高微球表面的氨基含量;然后利用自组装-化学镀法制备了SiO2@Au核壳填料,并对制备过程中反应溶液的pH值和甲醛用量进行了优化。场发射扫描电子显微镜表征结果显示,经过条件优化后制备的SiO2@Au核壳颗粒的表面Au包覆量较高,且包覆均匀、分散性较好。最后将谷胱甘肽(glutathione, GSH)分子修饰在SiO2@Au表面,条件优化后成功地制备了一种新型的两性离子型亲水色谱材料SiO2@Au-GSH,并将该填料填入毛细管中,制备了SiO2@Au-GSH两性离子型毛细管亲水色谱柱,并在毛细管液相色谱和加压毛细管电色谱系统中考察了色谱柱的亲水性能,研究证明SiO2@Au-GSH毛细管柱具有较好的分离能力和亲水性质。

关键词: SiO2@Au核壳填料, 谷胱甘肽, 加压毛细管电色谱, 聚乙烯亚胺, 毛细管亲水色谱柱, 毛细管液相色谱

Abstract:

In order to improve the contents of -NH2 group on the surface of SiO2, polyethylenimine (PEI) was introduced on the surface of SiO2 through Schiff Base reaction. Then self-assembled monolayer electroless plating (SAM-electroless plating) method was used to prepare SiO2@Au core-shell particles. During this process, two factors were discussed. They were the reaction pH in the SiO2@Au seed forming phase and the reaction volume of formaldehyde in the SiO2@Au seed growth phase. The scanning electronic microscopy (SEM) showed the coverage of Au was high and the dispersity was uniform after the optimizations. As we know, Au can coordinate with -SH group easily, so glutathione (GSH) can be bound on the surface of Au. In this study, GSH was bound on the surface of Au through the optimization of the reaction pH. The Fourier transform infrared spectrum showed that the GSH was bound on the surface of Au successfully at pH 3. At last, this packing material was packed into capillary column by slurry packing method to prepare SiO2@Au-GSH capillary columns, and the capillary liquid chromatography (cLC) mode was used to certify the hydrophilic property of this kind of column. In addition, this kind of column was certified to have a good separation ability of polar compounds in pressurized capillary electrochromatography (pCEC) mode.

Key words: capillary liquid chromatography (cLC), glutathione (GSH), polyethyleneimine (PEI), pressurized capillary electrochromatography (pCEC), SiO2@Au core-shell packing

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