Thermally Modulated Cationic Copolymer Brush on Monolithic Silica Rods for High-Speed Separation of Acidic Biomolecules
Thermally Modulated Cationic Copolymer Brush on Monolithic Silica Rods for High-Speed Separation of Acidic Biomolecules
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DOI：
10.1021/am302889j
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发表时间：
2013-02-27
影响因子：
9.5
通讯作者：
Okano, Teruo
中科院分区：
文献类型：
--
作者：
Nagase, Kenichi;Kobayashi, Jun;Okano, Teruo
通过表面引发原子转移自由基聚合（ATRP）制备了一种新型的温度响应性阳离子共聚物-聚（N-异丙基丙烯酰胺（IPAAm）-甲基丙烯酸二甲氨基乙酯（DMAEMA）-聚叔丁基丙烯酰胺（tBAAm））刷状接枝硅胶整体柱，用于高效的温度响应性阴离子交换色谱基质。通过将含有ATRP引发剂的甲苯溶液流入整体式二氧化硅棒柱中，将ATRP引发剂接枝在整体式二氧化硅棒表面上。将IPAAm、DMAEMA和tBAAm单体和CuCl/CuCl 2/Me 6 TREN（ATRP催化体系）溶解在2-丙醇中，并将反应溶液在25 ℃下泵入预先制备的引发剂改性的柱中16小时。通过X射线光电子能谱（XPS）、元素分析、扫描电子显微镜（SEM）观察和凝胶渗透色谱（GPC）测试，证实了在整体硅棒表面构建的共聚物刷结构。制备的整体硅胶棒柱，其特征在于通过色谱分析。的阳离子共聚物刷改性的整体硅胶棒柱能够分离腺苷核苷酸与较短的分析时间（4分钟）比热敏共聚物刷改性的硅胶珠填充柱，因为减少了整体支撑材料的扩散路径长度。这些结果表明，温敏性阳离子共聚物刷接枝整体硅胶棒柱制备的ATRP是一个有前途的工具，用于分析酸性生物活性化合物与显着短的分析时间。
Poly(N-isopropylacrylamide (IPAAm) co 2 (dimethylamino)ethylmethacrylate(DMAEMA)-co-tert-butylacrylamide (tBAAm)), a thermoresponsive-cationic-copolymer, brush-grafted monolithic-silica column was prepared through surface-initiated atom transfer radical polymerization (ATRP) for effective thermoresponsive anion-exchange chromatography matrices. ATRP-initiator was grafted on monolithic silica-rod surfaces by flowing a toluene solution containing ATRP initiator into monolithic silica-rod columns. IPAAm, DMAEMA, and tBAAm monomers and CuCl/CuCl2/Me6TREN, an ATRP catalytic system, were dissolved in 2-propanol, and the reaction solution was pumped into the preprepared initiator modified columns at 25 degrees C for 16 h. The constructed copolymer-brush structure on monolithic silica-rod surface was confirmed by X-ray photoelectron spectroscopy (XPS), elemental analysis, scanning electron microscopy (SEM) observation, and gel permeation chromatography (GPC) measurement of grafted copolymer. The prepared monolithic silica-rod columns were also characterized by chromatographic analysis. The cationic copolymer brush modified monolithic silica-rod columns were able to separate adenosine nucleotides with a shorter analysis time (4 min) than thermoresponsive copolymer brush-modified silica-bead-packed columns, because of the reduced diffusion path length of monolithic supporting materials. These results indicated that thermoresponsive cationic copolymer brush grafted monolithic silica-rod column prepared by ATRP was a promising tool for analyzing acidic-bioactive compounds with a remarkably short analysis time.