CAS Key Laboratory of Separation Sciences for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China.
Anal Chem. 2010 Jul 1;82(13):5447-54. doi: 10.1021/ac1003147.
An inorganic-organic hybrid monolithic capillary column was synthesized via thermal free radical copolymerization within the confines of a capillary using a polyhedral oligomeric silsesquioxane (POSS) reagent as the inorganic-organic hybrid cross-linker and a synthesized long carbon chain quaternary ammonium methacrylate of N-(2-(methacryloyloxy)ethyl)-dimethyloctadecylammonium bromide (MDOAB) as the organic monomer. The preparation process was as simple as pure organic polymer-based monolithic columns instead of using POSS as the nanosized inorganic-organic hybrid blocks (cross-linker) of the monolithic matrix. The pore properties and permeability could be tuned by the composition of the polymerization mixture. The characterization and evaluation results indicated that the synthesized MDOA-POSS hybrid monolith possessed the merits of organic polymer-based monoliths and silica-based monoliths with good mechanical and pH (pH 1-11) stabilities, which may be attributed to the incorporation of the rigid nanosized silica core of POSS. Column efficiencies of 223 000 and 50 000 N/m were observed in capillary electro-driven chromatography (CEC) and mu-HPLC, respectively. Peptides and standard proteins were baseline separated by this hybrid column in CEC and mu-HPLC, respectively, as well. The separation of bovine serum albumin (BSA) tryptic digest was also attempted to show its potential application in proteome analysis.
通过在毛细管内的热自由基共聚反应,使用多面体低聚倍半硅氧烷(POSS)试剂作为无机-有机杂化交联剂和合成的长碳链季铵甲基丙烯酸酯 N-(2-(甲基丙烯酰氧基)乙基)-二甲基十八烷基溴化铵(MDOAB)作为有机单体,合成了一种无机-有机杂化整体毛细管柱。该制备过程与纯有机聚合物基整体柱一样简单,而无需将 POSS 用作整体基质的纳米级无机-有机杂化块(交联剂)。聚合混合物的组成可以调节孔性能和渗透性。表征和评估结果表明,合成的 MDOA-POSS 杂化整体柱具有有机聚合物基整体柱和基于硅胶的整体柱的优点,具有良好的机械和 pH(pH 1-11)稳定性,这可能归因于刚性纳米尺寸的加入硅核心 POSS。在毛细管电动色谱(CEC)和微高效液相色谱(mu-HPLC)中观察到的柱效分别为 223000 和 50000N/m。该杂化柱还可在 CEC 和 mu-HPLC 中分别实现肽和标准蛋白质的基线分离。还尝试了牛血清白蛋白(BSA)胰蛋白酶消化物的分离,以显示其在蛋白质组分析中的潜在应用。