Department of Chemistry, Umeå University, Umeå, Sweden.
J Sep Sci. 2010 Oct;33(19):2965-76. doi: 10.1002/jssc.201000154.
A new method is presented for synthesizing a highly hydrophilic silica-based material for use in hydrophilic interaction chromatography. Porous silica particles used as a starting substrate were modified with 3-bromopropyl trichlorosilane and grafted with glycidyl methacrylate by controlled ("living") atom transfer radical polymerization in order to introduce an oxirane-carrying reactive tentacle layer on the silica surface. The grafted material was thereafter subject to an oxirane ring opening reaction with tris(hydroxy-methyl)aminomethane in dimethylformamide to yield a polymer-bound equivalent of the well known and highly hydrophilic "TRIS" buffering substance. Chemical characterization was done by diffuse reflectance FT-IR, X-ray photoelectron spectroscopy, elemental analysis, and (1)H NMR. Porosity and surface area examination was done with Brunauer-Emmett-Teller. Chromatographic application of the material was evaluated by separations of nucleic bases, small organic acids, and common nucleotides under mixed hydrophilic interaction chromatography and weak anion exchange conditions.
提出了一种新的方法来合成高度亲水的基于硅胶的材料，用于亲水相互作用色谱。用作起始底物的多孔硅胶颗粒先用 3-溴丙基三氯硅烷改性，然后通过受控（“活性”）原子转移自由基聚合接枝甲基丙烯酰氧基乙基三甲氧基硅烷，以在硅胶表面引入带有环氧的反应性触手层。接枝材料随后与三甲羟甲基氨基甲烷在二甲基甲酰胺中进行环氧开环反应，生成众所周知的高度亲水的“TRIS”缓冲物质的聚合物结合等效物。化学表征通过漫反射 FT-IR、X 射线光电子能谱、元素分析和（1）H NMR 进行。通过 Brunauer-Emmett-Teller 进行孔隙率和表面积检查。通过混合亲水相互作用色谱和弱阴离子交换条件下的核酸碱基、小有机酸和常见核苷酸的分离来评估该材料的色谱应用。
