原子转移自由基聚合法制备新型亲水开管毛细管柱及在毛细管电色谱上的应用  

Preparation of a novel hydrophilic open-tubular capillary column by surface initiated atom transfer radical polymerization and applications in capillary electrochromatography

作　　者：潘一廷[1,2] 马成[1,2] 白海红[1,2] 张养军[2] 秦伟捷[2] 钱小红[2] 

机构地区：[1]北京理工大学生命学院,北京100081 [2]蛋白质组学国家重点实验室,北京蛋白质组研究中心,北京放射与辐射医学研究所,北京102206

出　　处：《色谱》2013年第10期995-1000,共6页Chinese Journal of Chromatography

基　　金：国家重大科学计划项目(2013CB911204);国家重大科学仪器设备开发专项项目(2011YQ09000504);国家自然科学基金项目(21275005;21235001)

摘　　要：为了增加开管毛细管柱（OTCC）的相比，提高分离效率，发展了表面引发原子转移自由基聚合法（SI-ATRP）制备葡萄糖聚合物修饰的开管毛细管柱。通过扫描电镜观察，该开管柱内壁上修饰了三维波浪状聚合物，明显增加了内壁比表面积和相比。在pH3～11范围内，对含糖聚合物修饰的开管柱和空柱的电渗流进行了比较。修饰后开管柱的电渗流仅为空柱的1／2～1／3，且在pH6～11范围内保持平稳。稳定的电渗流保证了分离的重复性和稳定性。用该开管毛细管柱成功实现了小分子混合物（苯丙氨酸、胸腺嘧啶、腺苷、鸟苷、5-溴尿嘧啶、水杨酸）以及蛋白质大分子（核精核酸酶B、转铁蛋白和牛血清白蛋白）的有效分离，结果表明葡萄糖聚合物修饰的开管毛细管柱具有良好的重复性和稳定性。A novel type of glycopolymer brushes grafted open-tubular capillary column （OTCC） was developed for the polar compound separation. Briefly, the glycerol methacrylate （GMA） polymer brushes were grafted on the inner wall of OTCC by the surface initiated atom transfer radical polymerization （SI-ATRP）. Next, glucose was coupled to the side chains of the GMA polymer brushes to obtain the hydrophilic stationary phase （PGMA-N-Glucose）. The optimized SI-ATRP reaction conditions were GMA/CuCl/CuCl2/cyclohexanol system grafting at 25 ℃ for l h. After the glucose coupling, the column back pressure was about 3 585 kPa. The structure of the glycopolymer brushes on the inner surface of OTCC was characterized by scanning electron microscopy （SEM）. The glycopolymer grafting resulted in the formation of three-dimensional wave-like polymer structure on the inner surface of OTCC and largely increased the interior surface area. Therefore, improved column efficiency and loading capacity can be achieved. Under the optimized conditions, the electro osmotic flow （EOF） strength of the glycopolymer brushes grafted OTCC was obviously less than that of the bare column when the pH value of the mobile phase ranging from 3 to 11. Using the glycopolymer brushes grafted OTCC, the baseline separations of polar molecules and proteins were obtained without peak tailing. The future work will focus on the further development of the glycopolymer brushes for the highly polar compound separation, such as glycans and glycoproteins.

关 键 词：表面原子转移自由基聚合 毛细管电色谱 开管毛细管柱 糖聚合物 

分 类 号：O658[理学—分析化学]