色谱

色谱

• 研究简报 • 上一篇    下一篇

聚合物整体固定相的制备及条件优化

魏远隆1,2,邹娟娟1,2,杨长龙2,3,张庆合2,张维冰2,王风云1,李彤2   

  1. 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
  • 收稿日期:2004-04-12 修回日期:1900-01-01 出版日期:2005-05-30 发布日期:1988-09-25
  • 通讯作者: 张庆合
  • 基金资助:

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

WEI Yuanlong1,2, ZOU Juanjuan1,2, YANG Changlong2,3, ZHANG Qinghe2, ZHANG Weibing2, WANG Fengyun1, LI Tong2   

  1. 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
  • Received:2004-04-12 Revised:1900-01-01 Online:2005-05-30 Published:1988-09-25

PDF

606

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。

关键词: 孔尺寸分布, 条件优化 , 整体固定相, 制备

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.

Key words: condition optimization , pore size distribution, preparation, monolithic stationary phase