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Effects of terminal group and chain length on temperature-responsive chromatography utilizing poly(N-isopropylacrylamide) synthesized via RAFT polymerization

机译:通过筏聚合合成聚(N-异丙基丙烯酰胺)温度响应色谱法对温度响应色谱法的影响

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Poly( N -isopropylacrylamide) with two chain lengths (MW: ca. 5000, and ca. 20?000 g mol ~(?1) ) was synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization, using 2-dodecylsulfanylthiocarbonylsulfanyl-2-methyl propionic acid as the chain transfer agent. The derivatization of terminal dodecyl groups to maleimide groups was performed through the reduction of terminal trithiocarbonate moieties. These polymers were grafted onto aminopropyl silica using an activated ester–amine coupling method. Five types of polymer modified silica beads were prepared, i.e. , long chain length, short chain length, and mixed chain length functionalized with a dodecyl terminal group, and long chain length and short chain length with a maleimide terminal group. The surface properties of the modified polymer silica beads were evaluated by employing them as the stationary phase in HPLC setups and examining the temperature-dependent elution profiles of five steroids. The retention factor of steroids became smaller when the terminal dodecyl group was substituted with a maleimide group. A hydrophobic dodecyl moiety on the outermost surface strongly affected the retention of steroids, and the retention factor of steroids on short chains was larger than that on long chains below the lower critical solution temperature. These results indicate that the chain length and terminal functional group on the outermost surface of the polymer have a critical effect on the characteristics of polymer modified silica bead interfaces.
机译:使用2-十二烷基磺酰基硫羰基磺酰基(MW:Ca.5000和Ca.200,MW:Ca.5000和Ca.200,MW:Ca.5000和Ca.200 000g mol〜(α1)。 2-甲基丙酸作为链转移剂。通过减少末端三碳酸酯部分进行终末端十二烷基衍生至马来酰亚胺基团。使用活化的酯 - 胺偶联方法将这些聚合物接枝到氨基丙基二氧化硅上。制备五种类型的聚合物改性二氧化硅珠,即长链长度,短链长度和用十二烷末端基团官能化的混合链长度,具有马来酰亚胺末端组的长链长度和短链长度。通过将它们作为HPLC设置中的固定相和检查五种类固醇的温度依赖性洗脱曲线来评价改性聚合物二氧化硅珠的表面性质。当末端十二烷基被马来酰亚胺基团取代时,类固醇的保留因子变小。最外表面上的疏水十二烷基部分强烈影响类固醇的保留,短链上的类固醇的保留因子大于低链条低于临界溶液温度的长链。这些结果表明,聚合物最外表面上的链长和末端官能团对聚合物改性二氧化硅珠界面的特性具有临界作用。

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