Wang Jiabin, Wu Fangling, Xia Ruirui, Zhao Qi, Lin Xucong, Xie Zenghong
Institute of Food Safety and Environment Monitoring, Fuzhou University, Fuzhou, 350108, China; Institute of Biomedical and Pharmaceutical Technology, Fuzhou University, Fuzhou, 350002, China.
Institute of Biomedical and Pharmaceutical Technology, Fuzhou University, Fuzhou, 350002, China.
J Chromatogr A. 2016 Jun 3;1449:100-8. doi: 10.1016/j.chroma.2016.04.069. Epub 2016 Apr 26.
A novel strategy for rapidly fabricating ionic liquid (IL)-bonded multifunctional monolithic stationary phase has been developed by an in-situ polycondensation of urea-formaldehyde (UF) and a lab-made acylamino-functionalized IL (1-acetylamino-propyl-3-methylimidazolium bromide, [AAPMIm]Br). Two polycondensation processes of UF with 1-amino-propyl-3-methylimidazolium bromide or [AAPMIm]Br were evaluated. Several parameters including mass ratio of urea-formaldehyde, amount of [AAPMIm]Br, polycondensation time and reaction temperature were optimized, and the [AAPMIm]Br-bonded monolithic stationary phase could be rapidly synthesized in 10min with a satisfactory permeability and mechanical stability. Used for pressurized capillary electrochromatography (pCEC), a typical hydrophilic interaction (HI) retention could be obtained in the resultant [AAPMIm]Br-bonded monolith when the content of acetonitrile (ACN) in mobile phase exceeded 20%. Multiple retention mechanisms such as hydrophilic interaction (HI), hydrogen bond (HH), anion-exchange and cation-exclude interactions, were acheived in the [AAPMIm]Br-bonded monolith. Various polar compounds including phenols, benzoic acid and its homologues, and enkephalins have been well separated and thus demonstrated a satisfactory separation performance of the obtained monolith. A facile access is lighted for rapid preparation of ionic liquid-bonded monoliths with multiple retention mechanisms for pCEC.
通过尿素-甲醛(UF)与实验室自制的酰氨基官能化离子液体(1-乙酰氨基丙基-3-甲基咪唑溴盐,[AAPMIm]Br)原位缩聚反应,开发了一种快速制备离子液体(IL)键合多功能整体固定相的新策略。评估了UF与1-氨基丙基-3-甲基咪唑溴盐或[AAPMIm]Br的两种缩聚过程。对尿素-甲醛的质量比、[AAPMIm]Br的用量、缩聚时间和反应温度等几个参数进行了优化,[AAPMIm]Br键合整体固定相可在10分钟内快速合成,具有令人满意的渗透性和机械稳定性。用于加压毛细管电色谱(pCEC)时,当流动相中乙腈(ACN)含量超过20%时,在所得的[AAPMIm]Br键合整体柱中可获得典型的亲水相互作用(HI)保留。在[AAPMIm]Br键合整体柱中实现了多种保留机制,如亲水相互作用(HI)、氢键(HH)、阴离子交换和阳离子排斥相互作用。包括酚类、苯甲酸及其同系物和脑啡肽在内的各种极性化合物得到了很好的分离,从而证明了所得整体柱具有令人满意的分离性能。为快速制备具有多种保留机制的用于pCEC的离子液体键合整体柱提供了一条简便途径。