The organic-silica hybrid poly( POSS-co-AM )monolithic columns were prepared by in-situ polymerization process with octavinyl-T8-silsesquioxane( POSS)as a crosslinking agent and acrylamide( AM ) as monomer,tetrahydrofuran( THF ) as a porogenic agent and azobi-sisobutyronitrile( AIBN)as initiator. In order to optimize the properties,the composition of the polymerization mixture was investigated. The optimum preparation conditions were as follows:both the mass ratios of monomer to porogen and POSS to AM were 1.0:5.0;the mass fraction of the initiator( AIBN)was 0. 1%. With the help of POSS materials,homogeneous column bed and good permeability were obtained. The columns were used in capillary liquid chromatogra-phy( cLC)and pressurized capillary electrochromatography( pCEC)for the separation of mix-tures of amines,nucleosides,nitrobenzene amines. Satisfactory separations for these samples are achieved. The column is proved to be useful in both reversed-phase chromatography ( RPLC)and hydrophilic interaction chromatography( HILIC).%以丙烯酰胺（ AM）为单体，八乙烯基倍半硅氧烷（ POSS）为交联剂，偶氮二异丁腈（ AIBN）为引发剂，四氢呋喃（ THF）为致孔剂，通过原位聚合法制备了 poly（ POSS-co-AM）有机-无机杂化整体柱，并对各反应物的配比进行了优化。结果表明，当功能单体与致孔剂、POSS 与 AM 的质量比均为1．0：5．0，AIBN 的质量分数为0.1％时，杂化整体柱的柱效最高。无机材料的引入使整体柱结构均匀并具有良好的渗透性，该整体柱既能用于亲水色谱模式，也能用于反相色谱模式。将制备的整体柱用于毛细管液相色谱和加压毛细管电色谱分离核苷类、胺类、硝基苯胺类等化合物，获得了良好的效果。
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