Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
J Chromatogr A. 2013 Aug 9;1302:81-7. doi: 10.1016/j.chroma.2013.06.013. Epub 2013 Jun 15.
The present study described the preparation of a novel phosphate ester-bonded silica (PES) stationary phase based on "thiol-ene" click chemistry. The composition of the surface grafts of PES stationary phase was determined by elemental analysis and solid state (31)P MAS NMR. Due to its hydrophilic phosphate-ester groups and short hydrophobic alkyl chains, the PES stationary phase exhibited dual retention mechanism via complexation and hydrophobic interactions with phenols. Benefiting from this special interaction mechanism, the newly synthesized PES stationary phase showed better selectivity in the separation of phenols compared to commercial octadecylsilyl-bonded silica (C18) columns. Furthermore, the separations of 10 nucleosides and nucleobases on the PES stationary phase were achieved in both reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode.
本研究描述了一种新型的基于“硫醇-烯”点击化学的磷酸酯键合硅胶（PES）固定相的制备。通过元素分析和固态（31）P MAS NMR 确定了 PES 固定相表面接枝物的组成。由于其亲水性磷酸酯基团和短疏水性烷基链，PES 固定相通过与酚类物质的络合和疏水相互作用表现出双重保留机制。得益于这种特殊的相互作用机制，新合成的 PES 固定相对于酚类物质的分离具有更好的选择性，优于商业的十八烷基硅烷键合硅胶（C18）柱。此外，在反相液相色谱（RPLC）模式和亲水作用液相色谱（HILIC）模式下，均可实现 10 种核苷和碱基的分离。
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