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常规和极性嵌入 C16 硅胶整体固定相的胶束电动色谱性能。

Electrochromatographic performance of conventional and polar-embedded C16 silica monolithic stationary phases.

机构信息

Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education), College of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin, PR China.

出版信息

J Sep Sci. 2010 Nov;33(21):3386-92. doi: 10.1002/jssc.201000439.

Abstract

A novel monolithic silica column that has a polar-embedded amide-secondary amine group linking with C16 functionality for RP-CEC is described. The amide-secondary aminealkyloxysilane was synthesized by the reaction of 3-(2-aminoethylamino) propyltrimethoxysilane with hexadecanoyl chloride. Then, the silylant agent was bonded to the silica monolith matrix to produce hexadecanamide-secondary amine bonded silica (HDAIS) monolithic column. The electrochromatographic performance of HDAIS monolithic column for the separation of neutral, basic and polar solutes was studied, which was compared to that using the hexadecyl bonded silica monolithic column. The HDAIS monolithic column displayed reduced hydrophobic retention characteristics in the separation of five hydrophobic n-alkylbenzenes and four polar phenols when compared to the hexadecyl bonded silica monolithic column. A very much reduced silanol activity of HDAIS monolithic column was observed in the separation of test basic mixture including four aromatic amines, atenolol and metoprolol with 10 mM borate buffer (pH 7.5) containing 30% v/v ACN as the mobile phase. The comparison results indicate good performance for both polar and basic mixtures on HDAIS monolithic column in RP-CEC, and also show promising results for further applications.

摘要

一种新型整体式硅胶柱,具有极性嵌入酰胺-仲胺基团与 C16 功能基相连,用于反相胶束电动色谱。酰胺-仲胺烷氧基硅烷是通过 3-(2-氨乙基氨基)丙基三甲氧基硅烷与十六酰氯反应合成的。然后,将硅烷试剂键合到硅胶整体基质上,生成十六酰胺-仲胺键合硅胶(HDAIS)整体柱。研究了 HDAIS 整体柱对中性、碱性和极性溶质的胶束电动色谱分离性能,并与十六烷基键合硅胶整体柱进行了比较。与十六烷基键合硅胶整体柱相比,HDAIS 整体柱在分离 5 种疏水性正烷基苯和 4 种极性酚时表现出较低的疏水性保留特性。在以 10 mM 硼酸缓冲液(pH 7.5)含 30% v/v ACN 为流动相分离碱性测试混合物时,HDAIS 整体柱的硅醇活性明显降低,该混合物包括 4 种芳香胺、阿替洛尔和美托洛尔。比较结果表明,HDAIS 整体柱在反相胶束电动色谱中对极性和碱性混合物均具有良好的性能,也为进一步应用提供了有希望的结果。

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