混合模式毛细管聚合物整体柱的制备及应用

Preparation and application of mixed-mode capillary polymer monolithic column

混合模式毛细管整体色谱柱由于保留机理多样,具有很好的应用前景。本文以[2-(甲基丙烯酰基氧基)乙基]二甲基-(3-磺酸丙基)氢氧化铵(SPE)为单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为引发剂,正丙醇/1,4-丁二醇/水三元体系为致孔剂,制备了聚合物基质SPE-co-EDMA毛细管液相色谱整体柱。通过系统优化致孔剂和反应物种类和配比、引发剂的用量、反应时间和反应温度等因素,提高了整体柱的柱效、机械强度、渗透性和重复性。结果表明该毛细管整体柱在10 MPa内具有良好的机械强度,渗透性为2.17×10-14 m2,而且批次内和批次间峰面积的重现性(RSD)分别为1.0%和4.6%。以极性和非极性的多种化合物评价了该毛细管整体柱的色谱性能,结果表明该柱在高有机相中具有亲水相互作用机理,在低有机相中具有反相作用机理,显示出混合模式分离特性。

Based on the diversity of the retention mechanism ,mixed-mode capillary monolithic columns have broad application prospect. In this work,a novel capillary polymer monolithic column was prepared with [ 2-（ methacryloyloxy ）ethyl ]dimethyl-（ 3-sulfopropyl ）ammonium hydroxide（ SPE）as monomer,ethylene dimethacrylate（ EDMA）as crosslinking agent,azobi-sisobutyronitrile（ AIBN ） as initiator and butylalcohol/1,4-butanediol/water as ternary poro-gens. Under the optimized reaction conditions including the proportion of monomer and poro-gens,amount of initiator,reaction temperature and polymerization time,the monolithic col-umn showed good mechanical strength up to 10 MPa,high permeability of 2. 17 ＆#215; 10-14 m 2 and good repeatability. The peak area RSDs of column-to-column and batch-to-batch reproducibility were 1. 0% and 4. 6%,respectively. Finally,the capillary monolithic column was evaluated with polar and non-polar test mixtures. It showed hydrophilic interaction under high organic phase while hydrophobic interaction under low organic phase,indicating it a mixed-mode monolithic column.