聚(4-乙烯基苯硼酸-季戊四醇三丙烯酸酯)亲和整体柱的制备与应用

以4-乙烯基苯硼酸为单体,季戊四醇三丙烯酸酯为交联剂,偶氮二异丁腈为引发剂,乙二醇和二甘醇为致孔剂,经原位聚合制备了聚(4-乙烯基苯硼酸-季戊四醇三丙烯酸酯)毛细管整体柱.以单体、交联剂、致孔剂和引发剂的用量为4种因素,最大吸附量、柱效和保留时间为3个考察标准,利用实验设计软件(DOE)优化了其合成条件,验证了正交实验最优结果,得到了整体柱合成的最佳配比为单体7.32 mg,交联剂6 mg,致孔L剂100 μL,引发剂1 mg.在最佳条件下合成整体柱,并进行表征,在微径液相色谱(μHPLC)和加压毛细管电色谱(pCEC)实验中考察了分离特性.结果表明,整体柱固定相表面的硼酸基团在碱性条件下能特异性吸附邻苯二酚、腺苷等含有邻二羟基结构的化合物,具有亲和色谱的特性；同时由于交联剂的性质使其具有反相分离机理,在含有20％有机相的条件下能够将极性不同的苯系物分开.

Preparation, Characterization and Applications of Poly ( 4-vinylphenylboronic-co-pentaerythritol triacrylate) Affinity Monolithic Capillary Columns

A boronate functionalized monolithic capillary column was synthesized,characterized and utilized in the mode of both affinity and reversed phase chromatography.The polymer was prepared using 4-vinylphenylboronic acid as the functional monomer,pentaerythritol triacrylate as crosslinker,azobisisbutyronitrile as trigger,ethanediol and diethylene glycol as porogenator.In order to optimize the properties,the orthogonal experiment was designed by the DOE software.The optimum preparation conditions were monomer(4-vinylphenyl-boronic acid(VPBA),732 mg),cross-linking agent(pentaerythritol triacrylate(PETA),6 mg),trigger(azobisisobutyronitrile(AIBN),1 mg) and pore-foaming agent(diethylene glycol-ethanediol,2 ∶ 8,V/V).The column with the best proportion was characterized and applied in capillary high performance liquid chromatography(μHPLC) and pressurized capillary electrochromatography(pCEC).The results suggested the column persisted affinity chromatography character because the boronate group located at the stationary phase could specifically absorb compounds containing cis-dihydroxy functionality at alkaline conditions;because of the properties of PETA,the column also persist RP separation mechanism and separate different benzene series in 20 percent organic phase.