Dipartimento di Chimica e Tecnologie del Farmaco, Università degli Studi di Roma "La Sapienza", Piazzale Aldo Moro 5, 00185, Roma, Italy.
Dipartimento di Chimica e Tecnologie del Farmaco, Università degli Studi di Roma "La Sapienza", Piazzale Aldo Moro 5, 00185, Roma, Italy.
J Chromatogr A. 2022 Jul 19;1675:463173. doi: 10.1016/j.chroma.2022.463173. Epub 2022 May 22.
Modification of surface silanols is a topic of interest in the preparation of organo-functionalized silica particles. Herein, two novel contributions, mainly focused on separation science, were presented: i) the horizontal polymerization on silica surface by using the vinyl-triacetoxy silane and ii) a preparation of cysteine-based stationary phase via photo-click thiol-ene coupling. In the first derivatization step, the vinyl-triacetoxy silane was employed instead of conventional trichloro vinyl one. The one-step synthetic procedure needed imidazole as an activating agent in addition to the silica hydration. Modified silica particles offer a high loading of vinyl fragments and an extensive passivation of silanols such as to not require a subsequent end-capping procedure. The structural morphology of media was deeper characterized by combining infrared spectroscopy, solid-state nuclear magnetic resonance, and elemental analysis. A first application, the photo-click cysteine-based material was prepared by photo-click reaction and the stationary phase was employed in the separation of some conventional targets by hydrophilic interaction chromatography.
表面硅醇的修饰是制备有机功能化硅颗粒的研究热点。本文主要围绕分离科学提出了两项新的研究贡献：i）利用乙烯基三乙氧基硅烷在硅胶表面进行水平聚合；ii）通过光点击硫醇-烯加成反应制备半胱氨酸固定相。在第一步衍生化步骤中，使用乙烯基三乙氧基硅烷代替传统的三氯代乙烯基硅烷。一步法合成需要咪唑作为活化剂，此外还需要硅胶水合。改性硅胶颗粒具有较高的乙烯基片段负载量和广泛的硅醇封端，因此不需要进行后续的封端处理。通过结合红外光谱、固态核磁共振和元素分析对介质的结构形态进行了更深入的表征。首次应用是通过光点击反应制备基于半胱氨酸的光点击材料，并将固定相用于亲水作用色谱分离一些常规目标物。
