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聚合物整体固定相的制备及条件优化

Preparation and Optimization of Polymer-Based Monolithic Stationary Phase for High Performance Liquid Chromatography

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【作者】 魏远隆邹娟娟杨长龙张庆合张维冰王风云李彤

【Author】 WEI Yuanlong~ 1,2, ZOU Juanjuan~ 1,2, YANG Changlong~ 2,3, ZHANG Qinghe~2, ZHANG Weibing~2, WANG Fengyun~1, LI Tong~2 (1. Industrial Chemistry Institute, Nanjing University of Science and Technology, Nanjing 210094, China; 2. Dalian Elite Analytical Instrument Co. Ltd., Dalian 116011, China; 3. College of Chemical Engineering, Dalian University of Technology, Dalian 116024, China)

【机构】 南京理工大学工业化学研究所大连依利特分析仪器有限公司大连理工大学化工学院 江苏南京210094大连依利特分析仪器有限公司辽宁大连116011江苏南京210094大连依利特分析仪器有限公司辽宁大连116011大连理工大学化工学院辽宁大连116024江苏南京210094辽宁大连116024

【摘要】 采用无搅动原位聚合模式,在聚醚醚酮柱管中直接制备了聚合物整体固定相。通过扫描电镜观察到该整体固定相的孔径分布呈双峰模式,且孔结构均匀。用压汞法测定了该固定相的孔径分布、孔隙率及比表面积等参数,考察了致孔剂组成、聚合温度及交联剂含量等参数对固定相孔结构的影响,并对制备条件进行了优化。测定了流速与柱前压的关系,实验表明此整体固定相具有良好的通透性。通过对山羊血清和低聚核苷酸的分离分析,证明了所制备的整体固定相适合用于生物大分子的分离纯化。

【Abstract】 Unstirred in-situ polymerization was employed to directly produce glycidyl methacrylate-ethylene dimethacrylate copolymer (poly(GMA-co-EDMA) ) monoliths. Mercury intrusion method was adopted to measure some parameters of the monoliths, such as pore size distribution, porosity and specific surface area. Effects of key variables such as composition of pore-forming solvent mixture, temperature and content of cross-linking reagent, divinyl monomer on porous structure of monoliths were studied. The optimization of preparation conditions was achieved. Homogeneous micro porous structure was observed in the monoliths by scanning electron microscope. The effect of flow rate on back pressure was investigated, and good permeability of the monolithic stationary phase was obtained. The monolithic column was also used for the separation of goat serum and five oligonucleotides, and the results proved that the monolithic column is suitable for the separation of biopolymers.

【基金】 国家自然科学基金资助项目(No.20105006).
  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2005年03期
  • 【分类号】O657.7
  • 【被引频次】26
  • 【下载频次】232
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