Thermoresponsive polymer brush on monolithic-silica-rod for the high-speed separation of bioactive compounds.
Thermoresponsive polymer brush on monolithic-silica-rod for the high-speed separation of bioactive compounds.
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DOI：
10.1021/la201360p
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发表时间：
2011-07
期刊：
影响因子：
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通讯作者：
K. Nagase;J. Kobayashi;A. Kikuchi;Y. Akiyama;H. Kanazawa;T. Okano
中科院分区：
文献类型：
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作者：
K. Nagase;J. Kobayashi;A. Kikuchi;Y. Akiyama;H. Kanazawa;T. Okano
聚N-异丙基丙烯酰胺是目前应用最广泛的热敏聚合物之一，通过表面引发原子转移自由基聚合(ATRP)制备了刷子接枝的整体硅胶色谱柱。通过将含有ATRP引发剂的甲苯溶液注入到整体硅棒柱中，将ATRP引发剂接枝到整体硅棒表面。将N-异丙基丙烯酰胺(IPAAm)单体和ATRP催化体系CuCl/CuCl2/Me(6)Tren溶解在异丙醇中，将反应溶液泵入预制的引发剂改性柱中，在25℃下反应16h，通过XPS、元素分析、扫描电子显微镜观察和GPC测定证实了接枝的PIPAAm在整体硅棒表面形成了PIPAAm刷状结构。制备的整体硅胶棒柱也进行了色谱分析。与PIPAAm刷子修饰硅胶小球填充柱相比，PIPAAm刷子修饰的硅胶棒柱能够在较短的分析时间(10min)内分离疏水类固醇，这是因为整体支撑材料的扩散路径长度是水平受限的。此外，稀释的PIPAAm-刷子整体硅胶棒柱进一步缩短了分析时间(5min)。这些结果表明：(1)表面引发的ATRP在硅棒表面构建了PIPAAm-刷子结构；(2)ATRP制备的PIPAAm-刷子接枝硅胶棒柱是一种分析疏水生物活性物质的有效工具。
Poly(N-isopropylacrylamide), one of the most utilized thermoresponsive polymers, brush-grafted monolithic-silica columns were prepared through surface-initiated atom transfer radical polymerization (ATRP) for effective thermoresponsive-chromatography matrices. ATRP initiator was grafted on monolithic silica-rod surfaces by flowing a toluene solution containing ATRP initiator into monolithic silica-rod columns. N-Isopropylacrylamide (IPAAm) monomer and CuCl/CuCl(2)/Me(6)TREN, an ATRP catalytic system, were dissolved in 2-propanol, and the reaction solution was pumped into the preprepared initiator-modified columns at 25 °C for 16 h. The constructed PIPAAm-brush structure on the monolithic silica-rod surface was confirmed by XPS, elemental analysis, SEM observation, and GPC measurement of grafted PIPAAm. The prepared monolithic silica-rod columns were also characterized by chromatographic analysis. PIPAAm-brush-modified monolithic silica-rod columns were able to separate hydrophobic steroids with a short analysis time (10 min), compared to PIPAAm-brush-modified silica-beads-packed columns, because of the horizontally limited diffusion path length of monolithic supporting materials. Additionally, diluted PIPAAm-brush monolithic silica-rod column gave a further shorting analysis time (5 min). These results indicated (1) surface-initiated ATRP constructed PIPAAm-brush structures on monolithic silica-rod surfaces and (2) PIPAAm-brush grafted monolithic silica-rod column prepared by ATRP was a promising tool for analyzing hydrophobic-bioactive compounds with a short analysis time.