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制备和评价基于交联聚甲基丙烯酸缩水甘油酯的麦芽糖改性聚合物-二氧化硅复合材料作为高效液相色谱固定相。

Preparation and evaluation of maltose modified polymer-silica composite based on cross-linked poly glycidyl methacrylate as high performance liquid chromatography stationary phase.

机构信息

Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry & Molecular Engineering, East China University of Science and Technology, Shanghai, 200237, PR China.

Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry & Molecular Engineering, East China University of Science and Technology, Shanghai, 200237, PR China.

出版信息

Anal Chim Acta. 2018 Dec 7;1036:179-186. doi: 10.1016/j.aca.2018.06.027. Epub 2018 Jun 12.

Abstract

A new maltose modified polymer-silica composite was fabricated and applied as high performance liquid chromatography (HPLC) stationary phase. The cross-linked poly glycidyl methacrylate (pGMA) layer was chemically bonded to the outer surface as well as pore inner surface of silica beads via in-situ polymerization, and then maltose was modified onto the polymer layer via a [3 + 2] "click" reaction. The porous spherical silica (4 μm diameter) with 300 Å pore size was selected as the matrix so that the 3.25 nm-thick polymer layer fabricated on the pore inner surface would not affect its permeability. The typical 'U-shape' retention curves indicated a mixed-mode retention mechanism of the as-synthesized stationary phase. Both polar and non-polar analytes could be well separated on the stationary phase with column efficiency reaching 123809 plates/m for guanosine in hydrophilic interaction liquid chromatography (HILIC) mode and 46808 plates/m for fluorene in reversed-phase liquid chromatography (RPLC) mode, respectively. Nucleotides and their bases were baseline separated with good peak shape without any buffer salt in mobile phase, suggesting the effective shielding of the silanol groups. The packing material also showed excellent chromatographic repeatability with intraday RSDs of the retention time of five nucleosides less than 0.048% (n = 3) and interday RSDs less than 0.33% (n = 7) and great pH stability (from 1.5 to 10.2). Finally, the stationary phase was applied to the separation of ginseng extract.

摘要

一种新型的麦芽糖修饰聚合物-二氧化硅复合材料被制备出来,并作为高效液相色谱(HPLC)固定相应用。交联的聚缩水甘油甲基丙烯酸酯(pGMA)层通过原位聚合化学结合到二氧化硅珠的外表面和孔内表面上,然后通过[3+2]“点击”反应将麦芽糖修饰到聚合物层上。选择直径为 4μm、孔径为 300Å 的多孔球形二氧化硅作为基质,使得在孔内表面上制备的 3.25nm 厚的聚合物层不会影响其渗透性。典型的“U 形”保留曲线表明了所合成的固定相的混合保留机制。极性和非极性分析物都可以在固定相上得到很好的分离,在亲水作用色谱(HILIC)模式下,鸟嘌呤的柱效达到 123809 板/m,在反相液相色谱(RPLC)模式下,芴的柱效达到 46808 板/m。在流动相中没有缓冲盐的情况下,核苷酸及其碱基可以得到基线分离,峰形良好,表明硅醇基团得到了有效屏蔽。该填料还表现出出色的色谱重现性,五种核苷的保留时间日内 RSD 小于 0.048%(n=3),日间 RSD 小于 0.33%(n=7),并且具有很好的 pH 稳定性(pH 1.5 至 10.2)。最后,该固定相被应用于人参提取物的分离。

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