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制备和评价具有表面结合辛酰基-氨丙基部分的两亲性硅胶整体柱用于毛细管电色谱。

Preparation and evaluation of amphiphilic silica-based monolithic column having surface-bound octanoyl-aminopropyl moieties for capillary electrochromatography.

机构信息

Tianjin Key Laboratory for Modern Drug Delivery and High-Efficiency, School of Pharmaceutical Science and Technology, Tianjin University, Tianjin, P. R. China.

出版信息

Electrophoresis. 2010 Jun;31(12):1983-90. doi: 10.1002/elps.200900712.

DOI:10.1002/elps.200900712
PMID:20496345
Abstract

A novel amphiphilic silica-based monolithic column having surface-bound octanoyl-aminopropyl moieties was successfully prepared by a one-step in situ derivatization process. As expected, the amphiphilic monolithic column exhibited RP chromatographic behavior toward non-polar solutes (e.g., alkyl benzenes) with high column performance. As the pH of the buffer inside the column increases, the EOF changed from -2.65 x 10(-8) m(2) V(-1) s(-1) at pH 3.0 to 1.20 x 10(-8) m(2) V(-1) s(-1) at pH 8.0 with the reversion of EOF at about pH 6.4. Using acidic mobile phase, five aromatic acids can be efficiently separated in less than 6 min under co-EOF conditions. For basic compounds, symmetrical peaks were obtained due to the existence of hydrophilic acyl amide group, which can effectively minimize the adsorption of the positively charged basic analyte to the silica-based surface of the capillary column.

摘要

一种新型的基于两亲性硅的整体柱,其表面结合了辛酰基-氨丙基部分,通过一步原位衍生化过程成功制备。正如预期的那样,该两亲性整体柱对非极性溶质(如烷基苯)表现出反相色谱行为,具有较高的柱性能。随着柱内缓冲液 pH 的增加,EOF 从 pH 3.0 时的-2.65 x 10(-8) m(2) V(-1) s(-1)变为 pH 8.0 时的 1.20 x 10(-8) m(2) V(-1) s(-1),EOF 在 pH 6.4 左右反转。在共 EOF 条件下,使用酸性流动相,五种芳香酸可在不到 6 分钟内有效分离。对于碱性化合物,由于存在亲水性酰胺基团,可得到对称峰,这可有效减少带正电荷的碱性分析物对毛细管柱硅基表面的吸附。

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