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

作　　者：窦阿波[1] 邹存杰[2] 单圆鸿[1] 石先哲[1] 许国旺[1] 

机构地区：[1]中国科学院大连化学物理研究所中国科学院分离分析化学重点实验室,辽宁大连116023 [2]辽宁对外经贸学院,辽宁大连116052

出　　处：《色谱》2014年第5期447-451,共5页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(21275141)

摘　　要：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.

关 键 词：毛细管高效液相色谱 毛细管整体柱 制备 混合模式 

分 类 号：O658[理学—分析化学]