以二甲亚砜/正十二醇为二元致孔剂的新型苯乙烯-二乙烯苯毛细管整体柱的制备与表征

首次以二甲亚砜/正十二醇为二元致孔剂,苯乙烯为单体,二乙烯苯为交联剂,过氧化苯甲酰为引发剂,通过原位聚合反应制备了苯乙烯-二乙烯苯聚合物型毛细管整体柱。结果表明,苯乙烯∶二乙烯苯∶二甲亚砜∶正十二醇的体积比为18.7∶15.3∶13.2∶52.8,即二甲亚砜占致孔剂的比例为20%,交联度为45%,致孔剂含量为66%为最优配比。所合成的整体柱实现了反相色谱模式下对小分子苯系物与生物大分子蛋白的快速分离。其中蛋白分离实验的流速达到104μL·min-1,线速度约为12 mm·s-1,而常规色谱柱的线速度为1~2 mm·s-1。该整体柱的渗透性好,可用于物质的高速分离,若对其进行化学修饰,有望用于其它色谱分离模式。

Preparation and Characterization of a PS-DVB Monolithic Column Using Dimethylsulfoxide/Dodecanol as Binary Porogenic Agent

A novel styrene-divinylbenzene copolymer monolithic capillary column was prepared using dimethylsulfoxide/dodecanol as binary porogenic agent.The polymer was prepared with styrene as monomer,divinylbenzene as crosslinker,benzoperoxide as initiator.In order to optimize the properties,the contents of the polymerized mixtures were investigated.Key variables such as composition of porogenie agent and crosslinking degree and content of porogenic agent in the mixtures could be controlled easily during the on-column polymerization.The PS-DVB monolithic column was characterized by scan electric microscopy(SEM),inverse size exclusion chromatography (ISEC),and measured under back pressure at different flow rates to evaluate the porous properties.Homologous compounds of benzene and some proteins were used as objective probes in reverse phase chromatography mode for evaluating the separation performance of the synthesized column.The optimum preparation conditions were as follows:the volume ratio of styrene and divinylbenzene and dimethylsulfoxide and dodecanol was 18.7∶15.3 ∶ 13.2 ∶ 52.8,that is,the content of dimethylsulfoxide in binary porogenic agent occupied 20％,the degree of crosslinking tooked up to 45％ and the content of binary porogenic agent reached to 66％.The flow rate reached to 104 μL · min-1 in the experiment for the separation of protein,and the line speed was about 12 mm · s-1,while the conventional speed was about 1-2 mm · s-1 With the advantage of excellent chromatographic separation efficiency for biological macromolecules,the monolithic capillary column could be available in other separation modes if it is chemically modified.