色谱

色谱 ›› 2016, Vol. 34 ›› Issue (5): 467-472.DOI: 10.3724/SP.J.1123.2015.12040

• 研究论文 • 上一篇    下一篇

新型有机-无机杂化整体柱的制备及其在毛细管液相色谱及加压毛细管电色谱中的应用

翁中亚, 薛芸, 施文君, 王彦, 阎超   

  1. 上海交通大学药学院, 上海 200240
  • 收稿日期:2016-01-01 出版日期:2016-05-08 发布日期:2012-12-18
  • 通讯作者: 阎超, 王彦
  • 基金资助:

    国家自然科学基金项目(21175092);上海市科委科研计划项目(15142200200);上海市教育委员会科研创新项目(14YZ170);中国博士后科学基金项目(2015M581628).

Preparation of a new organic-silica hybrid monolithic column and its applications in capillary liquid chromatography and pressurized capillary electrochromatography

WENG Zhongya, XUE Yun, SHI Wenjun, WANG Yan, YAN Chao   

  1. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China
  • Received:2016-01-01 Online:2016-05-08 Published:2012-12-18
  • Supported by:

    National Natural Science Foundation of China (No. 21175092); Research and Development Program of Shanghai Municipal Science and Technology Commission (No. 15142200200); Innovation Program of Shanghai Municipal Education Commission (No. 14YZ170); China Postdoctoral Science Foundation Funded Project (No. 2015M581628).

PDF

100

被引次数

8

摘要：

以丙烯酰胺(AM)为单体,八乙烯基倍半硅氧烷(POSS)为交联剂,偶氮二异丁腈(AIBN)为引发剂,四氢呋喃(THF)为致孔剂,通过原位聚合法制备了poly(POSS-co-AM)有机-无机杂化整体柱,并对各反应物的配比进行了优化。结果表明,当功能单体与致孔剂、POSS与AM的质量比均为1.0: 5.0, AIBN的质量分数为0.1%时,杂化整体柱的柱效最高。无机材料的引入使整体柱结构均匀并具有良好的渗透性,该整体柱既能用于亲水色谱模式,也能用于反相色谱模式。将制备的整体柱用于毛细管液相色谱和加压毛细管电色谱分离核苷类、胺类、硝基苯胺类等化合物,获得了良好的效果。

关键词: 八乙烯基倍半硅氧烷, 丙烯酰胺, 加压毛细管电色谱, 毛细管液相色谱, 杂化整体柱

Abstract:

The organic-silica hybrid poly(POSS-co-AM) monolithic columns were prepared by in-situ polymerization process with octavinyl-T8-silsesquioxane (POSS) as a crosslinking agent and acrylamide (AM) as monomer, tetrahydrofuran (THF) as a porogenic agent and azobisisobutyronitrile (AIBN) as initiator. In order to optimize the properties, the composition of the polymerization mixture was investigated. The optimum preparation conditions were as follows: both the mass ratios of monomer to porogen and POSS to AM were 1.0: 5.0; the mass fraction of the initiator (AIBN) was 0.1%. With the help of POSS materials, homogeneous column bed and good permeability were obtained. The columns were used in capillary liquid chromatography (cLC) and pressurized capillary electrochromatography (pCEC) for the separation of mixtures of amines, nucleosides, nitrobenzene amines. Satisfactory separations for these samples are achieved. The column is proved to be useful in both reversed-phase chromatography (RPLC) and hydrophilic interaction chromatography (HILIC).

Key words: acrylamide (AM), capillary liquid chromatography (cLC), hybrid monoliths, octavinyl-T8-silsesquioxane (POSS), pressurized capillary electrochromatography (pCEC)

中图分类号: