色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1222-1229.DOI: 10.3724/SP.J.1123.2011.01222

• 研究论文 • 上一篇    下一篇

纤维素键合型手性整体柱的制备及其在快速手性分离中的应用

王家斌1, 王啸2, 李建华1, 吕海霞3, 林旭聪2, 谢增鸿2, 张其清1*   

  1. 1. 福州大学生物和医药技术研究院, 福建 福州 350002; 2. 福州大学食品安全与环境监测技术研究所, 福建 福州 350108; 3. 福州大学材料科学与工程学院, 福建 福州 350108
  • 收稿日期:2011-07-06 修回日期:2011-08-10 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 张其清,博士,教授,主要研究方向为功能高分子材料. Tel: (0591)87892016,
  • 基金资助:

    福建省科技厅重大专项(2010NZ0001-1)和福州大学科技发展基金项目(2010-XQ-17)

Preparation of chiral monolithic column with covalently bonded cellulose and their application to rapid enantioseparation

WANG Jiabin1, WANG Xiao2, LI Jianhua1, L Haixia3, LIN Xucong2, XIE Zenghong2, ZHANG Qiqing1*   

  1. 1. Institute of Biomedical and Pharmaceutical Technology, Fuzhou University, Fuzhou 350002, China; 2. Institute of Food Safety and Environmental Monitoring, Fuzhou University, Fuzhou 350108, China; 3. College of Materials Science and Engineering, Fuzhou University, Fuzhou 350108, China
  • Received:2011-07-06 Revised:2011-08-10 Online:2011-12-28 Published:2012-01-15

PDF

894

被引次数

16

摘要： 采用N-丙烯酰琥珀酰亚胺(NAS)为基质单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,原位聚合制备聚(NAS-co-EDMA)毛细管整体柱,并通过化学键合法将自合成的纤维素-三(4-甲基苯甲酸酯)(CTMB)共价键合到整体柱上,制备用于快速手性分离的纤维素键合型手性整体柱。优化了整体柱制备和衍生化条件;通过对固定相红外光谱和电渗流表征,证实CTMB已键合到整体柱上。探讨了流动相中乙酸浓度、甲醇含量等条件对整体柱手性分离的影响。使用该整体柱,分别在1.2 min内实现了5种对映体(苯丙氨酸、酪氨酸、色氨酸、普洛萘尔、苯乙醇)的毛细管电色谱快速手性分离,分离度可达1.31。

关键词: 共价键合, 快速手性分离, 毛细管电色谱, 手性毛细管整体柱, 纤维素-三(4-甲基苯甲酸酯)

Abstract: A chiral monolithic capillary column for rapid enantioseparation was prepared by covalently bonding of cellulose tris(4-methylbenzoate) (CTMB) on N-acryloxysuccinimide-based monolith. The preparation and derivatization conditions of the monolithic column were optimized. The successful grafting of CTMB was confirmed on the characterizations of the infrared spectrum and the cathodic electroosmotic flow (EOF). The effects of acetic acid concentration and methanol content on the enantioseparation were studied. The solvent resistance, reproducibility and stability of the monolithic column have also been investigated. The rapid enantioseparation of the five solutes (phenylalanine, tyrosine, tryptophan, propranolol and phenylethanol) with resolution (Rs) values up to 1.31 was achieved within 1.2 min on the prepared chiral capillary monolithic column by capillary electrochromatography.

Key words: chiral monolithic capillary column, covalent bonding, rapid enantioseparation, capillary electrochromatography (CEC), cellulose tris(4-methylbenzoate)