Huang Guihua, Zeng Wencan, Lian Qiuyan, Xie Zenghong
Department of Chemistry, Fuzhou University, Fuzhou, China.
J Sep Sci. 2008 Jul;31(12):2244-51. doi: 10.1002/jssc.200800009.
A novel silica monolithic stationary phase functionalized with 3-(2-aminoethylamino)propyl ligands for pressurized CEC has been presented. The monolithic capillary columns were prepared by a sol-gel process in 75 microm id fused-silica capillaries and followed by a chemical modification. The diamino groups on the surface of the stationary phase are meant to generate the chromatographic surface and a substantial anodic EOF as well as to provide electrostatic interaction sites for charged solutes. The electrochromatographic characterization and column performance were evaluated by a variety of neutral and charged solutes. It was observed that the anodic EOF for the diamine-bonded monolith was greatly affected by the reaction time with 3-(2-aminoethylamino)propyltrimethoxysilane and the PEG amount in the sol-gel reaction mixture in addition to the mobile phase conditions. The monolithic stationary phase exhibited hydrophilic interaction chromatographic behavior toward neutral solutes. Good separations of various solutes including phenols, nucleic acid bases, nucleosides and nucleotides were achieved under different experimental conditions. Fast and efficient separations were obtained with high plate counts reaching more than 130,000 plates/m.
本文介绍了一种用于加压毛细管电色谱的新型硅胶整体固定相,该固定相用3-(2-氨乙基氨基)丙基配体进行了功能化修饰。整体毛细管柱通过溶胶-凝胶法在内径75微米的熔融石英毛细管中制备,随后进行化学修饰。固定相表面的二氨基基团旨在产生色谱表面和可观的阳极电渗流,并为带电溶质提供静电相互作用位点。通过多种中性和带电溶质对电色谱特性和柱性能进行了评估。结果表明,除流动相条件外,二胺键合整体柱的阳极电渗流还受到与3-(2-氨乙基氨基)丙基三甲氧基硅烷的反应时间以及溶胶-凝胶反应混合物中聚乙二醇用量的显著影响。该整体固定相对中性溶质表现出亲水相互作用色谱行为。在不同实验条件下,实现了包括酚类、核酸碱基、核苷和核苷酸在内的各种溶质的良好分离。获得了快速高效的分离效果,塔板数高达130,000块/米以上。