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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Fast fabrication and modification of polyoctahedral silsesquioxane-containing monolithic columns via two-step photo-initiated reactions and their application in proteome analysis of tryptic digests
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Fast fabrication and modification of polyoctahedral silsesquioxane-containing monolithic columns via two-step photo-initiated reactions and their application in proteome analysis of tryptic digests

机译：通过两步光引发反应的快速制造和改性含聚昔德氏硅氧烷辛硅氧烷的整体柱及其在胰蛋白酶体缺口蛋白质组分析中的应用

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摘要

A fast and robust approach was developed to fabricate and modify hybrid monolithic columns via two-step photo-initiated reactions. At first, acrylopropyl polyoctahedral silsesquioxane (acryl-POSS) and 3-(triallyl silyl) propyl acrylate (TAPA) were chosen as precursors to synthesize poly (POSS-co-TAPA) monolithic column (monolith I) via photo-initiated free-radical polymerization within 10 min, which left lots of allyl groups on the surface of monolith. Secondly, two thiol-containing compounds, penicillamine and 1-octadecanethiol (ODT), were introduced to modify the prepared poly (POSS-co-TAPA) column via photo-initiated thiol-ene click reaction within 20 min. Finally, three resulting monolithic columns were applied to separate phenolic, anilines and antibiotics mixtures. These mixtures were baseline-separated on the monolith modified with penicillamine (monolith II), exhibiting better selectivity than both pristine monolith I and that modified with ODT (monolith HI). Additionally, these columns were further used for separation of tryptic digest of HeLa cells by cLC-MS/MS. The 5071 unique peptides mapped to 2442 proteins were identified from HeLa cells digest on monolith H, which were superior over those on monolith III, but slightly lower than those on monolith I. These results demonstrated that these POSS-containing columns exhibited great separation ability for complex samples.
机译：开发了一种快速且稳健的方法，以通过两步照片引发的反应制造和改性杂化整体柱。首先，选择丙烯丙基聚乙基二羟基硅氧烷（Acryl-POSS）和3-（三甲硅烷基）丙烯酸丙酯（TAPA）作为前体，以通过光引发的自由基合成聚（POSS-CO-TAPA）单片柱（全氧化钛I）在10分钟内聚合，在整料的表面上留下了大量的烯丙基组。其次，引入了两种含硫醇的化合物，青霉胺和1-十八烷基硫醇（ODT），以通过光引发的硫醇-NE键在20分钟内点击反应来改变制备的聚（POSS-COPA）柱。最后，将三个由此产生的单片柱施加到单独的酚醛，苯胺和抗生素混合物中。这些混合物在用青霉素（整甲硅II）的整体中是基线 - 分离，表现出比原始整料I和用ODT（整料HI）改性的选择性更好的选择性。另外，这些柱进一步用于通过CLC-MS / MS分离HeLa细胞的胰蛋白酶消化。从甲基HeLa细胞中鉴定为2442蛋白的5071个独特的肽，其在整料H上的含量优异，但略低于整料上的I.这些结果表明这些含有含量的柱表现出很大的分离能力复杂样品。

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