对-叔丁基杯[8]芳烃键合硅胶制备及其毛细管电色谱性能研究

高等学校化学学报 ›› 2005, Vol. 26 ›› Issue (7): 1228.

对-叔丁基杯[8]芳烃键合硅胶制备及其毛细管电色谱性能研究

李来生¹, 达世禄², 冯钰², 刘敏²

1. 南昌大学分析测试中心,南昌330047;
2. 武汉大学化学与分子科学学院,武汉430072

收稿日期:2004-08-26 出版日期:2005-07-10 发布日期:2005-07-10
通讯作者: 李来生(1962年出生),男,博士,教授,从事色谱及微分离技术研究.E-mail:lilaishengcn@163.com E-mail:lilaishengcn@163.com
基金资助:
江西省教委科技项目(批准号:JJ2003-73-16);江西省自然科学基金(批准号:9920024)资助

Preparation and Performance of p-tert-Butyl-calix[8]-arene-bonded Silica Gel for Capillary Electrochromatography

LI Lai-Sheng¹, DA Shi-Lu², FENG Yu-Qi², LIU Min²

1. Analytical and Testing Center, Nanchang University, Nanchang 330047, China;
2. College of Chemistry and Molecular Science, Wuhan University, Wuhan 430072, China

Received:2004-08-26 Online:2005-07-10 Published:2005-07-10

摘要/Abstract

摘要： 以γ-(环氧丙氧)丙基键合硅胶为前体,于硅胶表面键合环氧基,在催化剂存在下以杯芳烃钠盐开环制备杯芳烃键合硅胶固定相.该方法反应条件温和,适用性强.将这个新方法首次用于制备对-叔丁基杯[8]芳烃电色谱键合固定相(C8BS),采用加压电色谱初步评价其电色谱性能.研究结果表明,C8BS电渗流(Electrosmoticflow,EOF)较小,但通过控制键合反应及使用压力辅助电色谱可部分弥补上述不足.该固定相的EOF受流动相pH影响小(pH=3-8),同时大环配体屏蔽效应能有效地克服硅羟基引起的碱性化合物拖尾现象,这对电色谱分离具有重要意义.通过分步封尾研究EOF的来源发现,杯芳烃酚羟基对EOF有弱的贡献,这与报道的杯芳烃涂层具有径向电渗流调控能力相一致.

关键词: 杯芳烃键合硅胶固定相, 加压毛细管电色谱, 电色谱性能评价, 电渗流

Abstract: A new method for the preparation of calix-arene-bonded stationary phases(C8BS) was developed via the breaking epoxy group on the solid surface of the bonded 3-glycidoxypropyl silica by using active phenolic sodium of calix-arene in the presence of phase-transfer catalyst, which is moderate and universal. The new method was first introduced to the preparation of calixarene-bond stationary phase for capillary electrochromatography(CEC) with some modification. The new stationary phases were evaluated by the pressurized CEC(pCEC). The results show that the calixarene-bonding can provide lower and stable EOF over a wide pH range from 3-8, and the peak shapes of basic compounds on silica gel matrix can be improved because of the shield effect of the macrocyclic ligand, which are very important to CEC. Additionally, EOF source was studied by using silanization step by step. The result shows that the phenolic hydroxyl groups on the calixarene-bonded stationary phase result in EOF partially, which is consistent with the open-column of CEC reported.

Key words: Calixarene-bonded silica gel stationary phase, Pressurized capillary electrochromatography, Electrochromatographic evaluation, Electrosmotic flow

中图分类号:

O657

TrendMD:

李来生, 达世禄, 冯钰, 刘敏. 对-叔丁基杯[8]芳烃键合硅胶制备及其毛细管电色谱性能研究. 高等学校化学学报, 2005, 26(7): 1228.

LI Lai-Sheng, DA Shi-Lu, FENG Yu-Qi, LIU Min. Preparation and Performance of p-tert-Butyl-calix[8]-arene-bonded Silica Gel for Capillary Electrochromatography. Chem. J. Chinese Universities, 2005, 26(7): 1228.

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