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Macro-mesoporous organosilica monoliths with bridged-ethylene and terminal-vinyl: high-density click functionalization for chromatographic separation
Analytica Chimica Acta ( IF 6.2 ) Pub Date : 2018-12-01 , DOI: 10.1016/j.aca.2018.07.004
Ci Wu , Yu Liang , Xudong Zhu , Qun Zhao , Fei Fang , Xiaodan Zhang , Zhen Liang , Lihua Zhang , Yukui Zhang

A novel kind of macro-mesoporous organosilica monolith, with not only bridged-ethylene groups incorporated into the skeleton but also terminal-vinyl groups protruded from the pore-wall, was prepared so that high-loaded double bonds were achieved. Via highly efficient "thiol-ene" click reaction of such high-loaded double bonds, the surface coverage of C18 groups on monolith could be 5.54 μmol m-2, significantly larger than that of the reported separation materials, beneficial to improvement of separation resolution, especially for peptide separation. The separation performance was evaluated using alkylbenzenes and standard peptides. Furthermore, the tryptic digests of complex sample was successfully analyzed. Because of high separation resolution of our prepared hybrid monolith, the peak capacity for 6-h gradient was achieved as 482. Coupling to LTQ Orbitrap Velos Mass Spectrometry, 22523 tryptic peptides from 4423 proteins were identified from the HeLa cells, more than that using the other long-gradient separation by the same system reported, showing great promising of such monolith for large-scale in-depth proteomic analysis.

中文翻译:

具有桥连乙烯和末端乙烯基的大介孔有机硅整体料:用于色谱分离的高密度点击功能化

制备了一种新型的大介孔有机硅整料,不仅将桥接的乙烯基结合到骨架中,而且还从孔壁突出了末端乙烯基,从而实现了高负载双键。通过这种高负载双键的高效“硫醇-烯”点击反应,C18基团在整体上的表面覆盖率为5.54 μmol m-2,明显大于报道的分离材料,有利于提高分离分辨率,尤其适用于肽段分离。使用烷基苯和标准肽评估分离性能。此外,成功分析了复杂样品的胰蛋白酶消化物。由于我们制备的混合整体的高分离分辨率,6 小时梯度的峰容量达到 482。
更新日期:2018-12-01
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