基于SI-ATRP技术制备接枝聚乙烯基四唑色谱固定相及性能研究

Preparation of Poly(vinyltetrazole) Chain-grafted Chromatographic Stationary Phase by Surface-initiated Atom Transfer Radical Polymerization and Its Chromatographic Properties

应用表面引发原子转移自由基聚合技术(SI-ATRP),以合成的功能单体乙烯基四唑(VT)为单体,以自制的6.0μm单分散大孔交联聚甲基丙烯酸环氧丙酯(PGMA/EDMA)微球为基质,合成了新型弱阳离子交换并具有亲水作用的色谱固定相填料。控制VT单体与引发剂的比率,得到了接枝密度和链长可控的接枝聚乙烯基四唑(PVT)固定相。并考察了聚合反应过程,单体的合成与表征,弱阳离子交换性能、亲水性能等方面。实验结果表明,该色谱固定相色谱性能良好。

A novel stationary phase for weak cation exchange （WCX） and hydrophilic interaction chromatography （HILIC） was prepared with surface-initiated atom transfer radical polymerization （SI-ATRP）. Vinyltetrazole was grafted onto the surface of the beads in water medium with the polyglycidylmethacrylate beads （P（GMA/EDMA）） previously modified with 2-bromoisobutryl bromide as the macromolecule initiators and CuC1 as catalyst. The poly（vinyltetrazole）-grafted beads obtained with different atom transfer radical polymerization （ATRP） formulations were tried as chromatographic packings in ion-exchange chromatography. The results showed that the prepared columns could separate the tested proteins with high efficiency and high capacity, and the retention time of protein had a positive relationship with increasing the chain lengths of the grafted poly（vinyltetrazole） （PVT）. The prepared column was also found to be able to separate nucleosides by hydrophilic interaction chromatographic mode.