摘要
合成一种了氨基酸衍生物:4,4'-二苯亚甲基桥联-二[2-(1-咪唑基)-3-苯基丙醇氨基甲酸酯](ImPh-Carb),并将其键合到硅胶上制备了一种新的氨基甲酸酯功能化的离子液体HPLC固定相(ImPh-Carb-Silica)。利用1H NMR、13C NMR、MS和FTIR对ImPh-Carb进行了表征;通过FTIR和元素分析对ImPh-Carb-Silica固定相进行了表征,根据N含量计算得到ImPh-Carb-Silica的键合量为0.19 mmol/g。以5种芳烃、5种酚类化合物和4种有机磷农药为分析物,分别在正相和反相色谱模式下对固定相的色谱分离性能进行了评价,同时考察了流动相的变化与溶质保留因子lg k之间的关系。结果表明,该固定相与溶质分子间存在多重作用力,如疏水、氢键、π-π和偶极-诱导偶极作用等,使其能同时在正相和反相色谱模式下使用;在正相色谱条件下固定相对酚类化合物和有机磷农药表现出较好的分离选择性。
A new carbamate functionalized ionic liquid stationary phase(ImPh-Carb-Silica) for high-performance liquid chromatography was prepared by bonding 4,4′-diphenylmethylene-bis[2-(1-imidazolyl)-3-phenyl-1-propanol carbamate](ImPh-Carb) onto silica particles. The structure of ImPh-Carb was characterized by 1H NMR,13C NMR, MS and FTIR, and the bonded stationary phase was also characterized by FTIR and element analysis, and the bonding amount of ImPh-Carb-Silica stationary phase was about 0.19 mmol/g, according to the nitrogen content. The chromatographic performances of the stationary phase were evaluated using aromatic hydrocarbons, phenols and organophosphorus pesticides as solutes in reversed-phase and normal-phase chromatographic modes, and the effect of the content of mobile phase on retention factor(lg k) of analytes was studied. The results show that the functionalized ionic liquid stationary phase provides a multiple-interaction mechanism with analytes including hydrophobic, hydrogen bonding, π-π, and dipole-induce/dipole interactions. The stationary phase can be simultaneously performed in reversed-phase and normal-phase chromatographic modes, and it demonstrates its superiority in separation of phenols and organophosphorus pesticides under normal-phase chromatographic mode.
出处
《应用化学》
CAS
CSCD
北大核心
2013年第6期710-715,共6页
Chinese Journal of Applied Chemistry
基金
国家自然科学基金(20902017
2090520)
河南省科技创新杰出青年基金
郑州市科技攻关项目(083SGYG25121-11)资助
关键词
氨基甲酸酯功能化离子液体
固定相
高效液相色谱
多重作用机制
carbamate functionalized ionic liquid stationary phase high-performance liquid chromatography multiple-interaction mechanism