Department of pharmacy, Jiangxi University of Traditional Chinese Medicine, Nanchang, P. R. China.
J Sep Sci. 2021 Feb;44(3):735-743. doi: 10.1002/jssc.202000978. Epub 2020 Dec 17.
Hydroxypropyl-β-cyclodextrin-encapsulated stationary phase incorporated on silica monolith particles was prepared by physical embedding, providing a new method for the development of chiral stationary phase for enantioseparation in liquid chromatography. Ground silica monolith particles of about 2.0 μm were prepared via sol-gel reaction followed by differential sedimentation. Initially, the silica monolith particles were pretreated with 3-trimethoxysilyl propyl methacrylate to attach double-bonded ligands onto the surface, then a network structure was formed onto the surface of the particle using N-isopropyl acrylamide as functional monomer. Hydroxypropyl-β-cyclodextrin was encapsulated inside N-isopropyl acrylamide copolymerized layer on the surface of silica monolith particles. The effect of the amount of chiral selector on the chromatographic efficiency of the chiral stationary phase was examined. The glass lined stainless steel columns (1 mm internal diameter, 300 mm length) were packed with the stationary phase for estimation of the efficiency by separation of phenylsuccinic acid, oxybutynin, equol, and naproxen enantiomers in high-performance liquid chromatography, with the resolutions of 1.54, 1.72, 2.54, and 2.31, respectively. The column to column repeatabilities through relative standard deviation were found better than 3%. The experimental results indicate that the sol-gel ground silica particles modified with β-cyclodextrin provide a promising way for the separation of chiral enantiomers.
羟丙基-β-环糊精包埋的固定相通过物理嵌入法固定在硅胶整体柱颗粒上，为手性固定相在液相色谱中的对映体分离提供了一种新的发展方法。通过溶胶-凝胶反应和差速沉降制备粒径约为 2.0 μm 的硅胶整体柱颗粒。首先，用 3-三甲氧基硅丙基甲基丙烯酸酯对硅胶整体柱颗粒进行预处理，在表面上连接双键配体，然后用 N-异丙基丙烯酰胺作为功能单体在颗粒表面形成网络结构。羟丙基-β-环糊精被包裹在硅胶整体柱颗粒表面的 N-异丙基丙烯酰胺共聚层内。考察了手性选择剂的用量对手性固定相色谱效率的影响。采用玻璃内衬不锈钢柱（内径 1mm，长 300mm）填充固定相，通过高效液相色谱法分离苯琥酸、奥昔布宁、雌马酚和萘普生对映体，评估其效率，分辨率分别为 1.54、1.72、2.54 和 2.31。通过相对标准偏差发现柱间重复性较好，优于 3%。实验结果表明，β-环糊精修饰的溶胶-凝胶研磨硅胶颗粒为手性对映体的分离提供了一种有前途的方法。
