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【文摘发布】用于毛细管电色谱法和毛细管液相色谱法的一种分子印迹聚合物衍生的硅胶整

Title: Preparation and Evaluation of a Molecularly Imprinted Polymer Derivatized Silica Monolithic Column for Capillary Electrochromatography and Capillary Liquid Chromatography

Author:Junjie Ou, Xin Li, Shun Feng, Jing Dong, Xiaoli Dong, Liang Kong, Mingliang Ye, and Hanfa Zou

Resource: Analytical Chemistry, 2007,79 (2):639-646.

Abstract:A method for preparation of molecularly imprinted polymer (MIP) derivatized onto the surface of a monolithic silica capillary column was successfully developed. The vinyl groups were first introduced onto the silica monolith by immobilization of -methacryloxypropyltrimethoxysilane. Then the MIP coating was copolymerized and anchored onto the surface of the silica monolith. Acetonitrile was selected as porogen (solvent). The other preparation conditions, such as monomer concentration, temperature, and time of polymerization, were systematically studied. The obtained MIP-derivatized silica monolith using L-tetrahydropalmatine (L-THP) and (5S,11S)-(-)-Tröger's base (S-TB) as the imprinted template, respectively, was characterized in terms of the retention behavior of thiourea and toluene. Under the optimized CEC conditions, baseline enantioseparations of THP and TB were achieved in 4 min though the effective length of the columns was 8.5 cm. The result indicates that enough recognition sites were on the surface of silica monolith, resulting in strong recognition ability. Compared with a MIP organic monolith, the MIP-derivatized silica monolith exhibits better column efficiency and stability in CEC. Additionally, the comparison of these two kinds of monolithic columns was performed by capillary liquid chromatography. The separation on MIP-derivatized silica monolith was superior to that on the organic monolith.

PMID: 17222031
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题目:一种可用于毛细管电色谱和毛细管液相色谱的分子印迹聚合物衍生硅胶整体柱的制备与评价
作者:欧俊杰(音),……,邹汉法
文章来源:分析化学 2007,79 (2):639-646.

摘要:本文成功研究出一种新型毛细管色谱柱的制备方法,该硅胶整体柱表面键合有分子印迹聚合物。首先通过将3-甲基丙烯基氧丙基化三甲氧基硅烷固定在硅胶整体柱表面引入烯基官能团。然后分子印迹化合物通过与硅胶整体柱上的烯基发生共聚反应从而固定在其表面。选择乙腈为成孔剂(溶剂)。本文还对其它制备条件,比如单体浓度,温度,聚合反应时间都进行了系统研究。分别制备了以L-延胡索乙素(L-THP)和(5S,11S)-(-)-Tröger's碱(TB)为印迹模板的分子印迹聚合物衍生硅胶整体柱,并对硫脲和甲苯在柱上的保留行为进行了研究。在毛细管电色谱条件优化后,THP和TB的对映体在仅有8.5cm柱长的毛细柱上4min内就实现了基线分离。这一结果表明硅胶整体柱表面的位点识别能力很强。当应用于毛细管电色谱时,与分子印迹有机整体柱相比,分子印迹聚合物衍生硅胶整体柱表现出更佳的柱效和稳定性。此外,还在毛细管液相色谱条件下比较了这两种整体柱的表现。在分子印迹聚合物衍生硅胶整体柱表现仍然好于分子印迹有机整体柱。(丁香)
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