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Polyhedral Oligomeric Silsesquioxane as a Cross-linker for Preparation of Inorganic-Organic Hybrid Monolithic Columns

机译:多面体低聚倍半硅氧烷作为交联剂,用于制备无机-有机杂化整体柱

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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)-dimethy-loctadecylammonium 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.
机译: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N甲基丙烯酸季铵盐,通过毛细管内的热自由基共聚反应合成了无机-有机杂化整体毛细管柱。 -(2-(甲基丙烯酰氧基)乙基)-二甲基-十五烷基溴化铵(MDOAB)作为有机单体。制备过程就像使用纯有机聚合物基整体柱一样简单,而不是将POSS用作整体基质的纳米级无机-有机杂化嵌段(交联剂)。孔的性质和渗透性可以通过聚合混合物的组成来调节。表征和评价结果表明,合成的MDOA-POSS杂化整体具有有机聚合物基整体和二氧化硅基整体的优点,具有良好的机械稳定性和pH(pH 1-11)稳定性,这可能是由于掺入了聚合物。 POSS的刚性纳米二氧化硅芯。在毛细管电色谱法(CEC)和mu-HPLC中,柱效分别为223 000和50 000 N / m。肽和标准蛋白也分别通过该杂化柱在CEC和mu-HPLC中进行基线分离。还尝试分离牛血清白蛋白(BSA)胰蛋白酶消化物,以显示其在蛋白质组分析中的潜在应用。

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