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基于交替共聚物接枝硅胶的高选择性 HPLC 填充材料的制备。

Preparation of high-selective HPLC packing materials based on alternating copolymer-grafted silica.

机构信息

Department of Applied Chemistry and Biochemistry, Faculty of Engineering, Kumamoto University, Kumamoto, Japan.

出版信息

J Sep Sci. 2010 Oct;33(19):2977-89. doi: 10.1002/jssc.201000293.

Abstract

Three alternating copolymer-grafted silica stationary phases for use in high-selective RP-HPLC were prepared from two vinyl monomers selected from styrene, N-methylmaleimide, N-octadecylmaleimide, and octadecyl acrylate; they were characterized by elemental analyses, thermogravimetric analysis, diffuse reflectance infrared Fourier transform spectroscopy, and (13)C cross-polarization magic-angle spinning NMR spectroscopy. Aspects of molecular-shape selectivity were evaluated for three different columns using Standard Reference Material 869b, Column Selectivity Test Mixture for Liquid Chromatography. The best selectivity for isomer separations was obtained for the stationary phase prepared with a copolymer of octadecyl acrylate and N-octadecylmaleimide, which was able to separate 16 polycyclic aromatic hydrocarbons (Standard Reference Material 1647e) in an isocratic elution. In this paper, the effectiveness of this phase is also demonstrated by separation of tocopherol isomers.

摘要

三种用于高选择性反相高效液相色谱的交替共聚物接枝硅胶固定相,是由苯乙烯、N-甲基马来酰亚胺、N-十八烷基马来酰亚胺和十八烷基丙烯酸酯这两种乙烯基单体中选择两种制备的;它们的结构通过元素分析、热重分析、漫反射红外傅里叶变换光谱和(13)C 交叉极化魔角旋转 NMR 光谱进行了表征。使用液相色谱标准参考物质 869b 和柱选择性测试混合物对三种不同的色谱柱的分子形状选择性进行了评估。对于用十八烷基丙烯酸酯和 N-十八烷基马来酰亚胺共聚体制备的固定相,异构体分离的选择性最好,能够在等度洗脱条件下分离 16 种多环芳烃(标准参考物质 1647e)。本文还通过分离生育酚异构体证明了这种固定相的有效性。

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