Lv Yongqin, Hughes Timothy C, Hao Xiaojuan, Hart Noel K, Littler Stuart W, Zhang Xiaoqing, Tan Tianwei
College of Life Science and Technology, Beijing University of Chemical Technology, Beisanhuan East Road 15#, Beijing, 100029, China; Molecular and Health Technologies, CSIRO, Melbourne, 3169, Australia.
Macromol Rapid Commun. 2010 Oct 18;31(20):1785-90. doi: 10.1002/marc.201000345.
The copolymer poly(isocyanatoethyl methacrylate-co-methyl methacrylate-co-ethylene glycol dimethacrylate) (poly(IEM-co-MMA-co-EGDMA)) was developed as a novel, facile, highly reactive and versatile monolithic matrix, which was amenable to surface functionalization with a variety of nucleophilic modifiers based on the reactive isocyanate group, producing monoliths of various chemistries suitable for chromatography. The specific surface area, pore size distribution, porosity and morphology of the monolithic matrix were characterized using a mercury intrusion porosimeter and scanning electron microscopy (SEM), respectively. Thermal analysis results revealed that the monolith was thermally stable up to 307 °C. The success of the chemical modification of the monolithic matrix was confirmed by FT-IR, solid state (13) C NMR and XPS elemental analysis, showing the high ligand density of the modified monoliths. A ligand density of up to 2.33 mmol·mL(-1) was obtained for the 1-octanol modified monolith (M1) with an isocyanate group conversion of 96.9%, indicating a high efficiency of the modification reaction. The potential application of the monoliths was demonstrated by the separation of a series of compounds. The novel monolithic columns exhibited high mechanical stability, column efficiency and good repeatability and reproducibility.
共聚物聚（甲基丙烯酸异氰酸乙酯 - 甲基丙烯酸甲酯 - 乙二醇二甲基丙烯酸酯）（聚（IEM - co - MMA - co - EGDMA））被开发为一种新型、简便、高反应性且通用的整体基质，基于反应性异氰酸酯基团，它易于用多种亲核改性剂进行表面功能化，从而制备出适用于色谱分析的具有各种化学性质的整体柱。分别使用压汞仪和扫描电子显微镜（SEM）对整体基质的比表面积、孔径分布、孔隙率和形态进行了表征。热分析结果表明，该整体柱在高达307°C的温度下具有热稳定性。通过傅里叶变换红外光谱（FT - IR）、固态（13）C核磁共振（NMR）和X射线光电子能谱（XPS）元素分析证实了整体基质化学改性的成功，表明改性整体柱具有高配体密度。对于1 - 辛醇改性的整体柱（M1），异氰酸酯基团转化率为96.9%，配体密度高达2.33 mmol·mL(-1)，表明改性反应效率高。通过一系列化合物的分离证明了整体柱的潜在应用。新型整体柱表现出高机械稳定性、柱效以及良好的重复性和重现性。
