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聚苯乙烯固载溶胶-凝胶整体硅胶微球的一锅反应法提高分离效率。

Polystyrene Immobilized Sol-Gel Ground Silica Monolith Particles Using One-Pot Reaction of Enhanced Separation Efficiency.

机构信息

Department of Pharmacy, Jiangxi University of Traditional Chinese Medicine, Nanchang 330004, China.

出版信息

J Chromatogr Sci. 2021 Oct 29;59(10):949-955. doi: 10.1093/chromsci/bmab032.

Abstract

The stationary phase based on sol-gel ground silica monolith particles has been produced by one-pot polymerization method incorporation of styrene and ethylene dimethacrylate. First, the ground silica monolith particles were prepared by a sol-gel process followed by sedimentation. The particles were then subjected to modify with styrene ligand via one-pot polymerization, whereas ethylene dimethacrylate was used as the cross-linker. The glass lined stainless steel columns (1 mm internal diameter, 150 mm length) were packed with the above phase for estimation of the chromatographic performance in high-performance liquid chromatography. An average number of theoretical plates of as high as 39,300 plates/column was obtained under the optimized elution condition. The column-to-column reproducibility was proved satisfactory in separation efficiency and retention factor. The experimental results indicate that sol-gel ground silica particles prepared by an aid of one-pot modification can provide a better way for preparation of highly efficient stationary phase.

摘要

基于溶胶-凝胶法制备的硅胶整体颗粒的固定相是通过一步聚合方法将苯乙烯和乙二醇二甲基丙烯酸酯引入到硅胶整体颗粒中制备而成。首先,通过溶胶-凝胶工艺制备硅胶整体颗粒,然后通过沉降进行分离。然后,颗粒通过一步聚合与苯乙烯配体进行改性,而乙二醇二甲基丙烯酸酯则用作交联剂。将上述相填充到玻璃衬里不锈钢柱(内径 1mm,长度 150mm)中,以评估在高效液相色谱中的色谱性能。在优化的洗脱条件下,获得了高达 39300 块/柱的理论板数。在分离效率和保留因子方面,柱间重现性令人满意。实验结果表明,通过一步修饰制备的溶胶-凝胶法制备的硅胶颗粒可以为制备高效固定相提供更好的方法。

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