色谱

色谱

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酯型十八烷基键合硅胶整体柱的制备、表征及性能评价

王利娟1,杨更亮1,2,李煦1,李晓瑜1,尹俊发2,李志伟1,2,高文惠3,杨静4,陈义2

  

  1. 1. College of Pharmacy, Hebei University, Baoding 071002, China; 2. Molecular Science Center, Institute of Chemistry, The Chinese Academy of Sciences, Beijing 100087, China; 3. College of Biological Science and Engineering, Hebei University of Science and Technology, Shijiazhuang 050018,
    China; 4. China Institute of Atomic Energy, Beijing 102413, China
  • 收稿日期:2005-05-19 修回日期:2005-09-02 出版日期:2005-09-30 发布日期:1988-03-25
  • 通讯作者: 杨更亮

Synthesis, Characterization and Evaluation of Octadecyl Ester-Bonded Monolithic Column

WANG Lijuan1, YANG Gengliang1,2, LI Xu1, LI Xiaoyu1, YIN Junfa2, LI Zhiwei1,2, GAO Wenhui3, YANG Jing4, CHEN Yi2   

  1. 1. College of Pharmacy, Hebei University, Baoding 071002, China; 2. Molecular Science Center, Institute of Chemistry, The Chinese Academy of Sciences, Beijing 100087, China; 3. College of Biological Science and Engineering, Hebei University of Science and Technology, Shijiazhuang 050018,
    China; 4. China Institute of Atomic Energy, Beijing 102413, China
  • Received:2005-05-19 Revised:2005-09-02 Online:2005-09-30 Published:1988-03-25

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摘要：

将硅烷偶联剂γ-(2,3-环氧丙氧)丙基三甲氧基硅烷与十八酸反应,再键合到硅胶整体柱上,得到了酯型十八烷基键合固定相,并用红外光谱、元素分析对其进行了表征。在以甲醇-水为流动相的反相色谱条件下分离了苯、联苯和蒽的混合样品,评价了该整体柱的色谱性能,考察了该整体柱适用的pH范围,以及柱压降、柱效与流速的关系。结果表明,该硅胶整体柱键合效果良好,具有较好的反相色谱性能,且在pH=2～8时稳定性好,柱压降、柱效受流速影响较小,可有效地用于化合物的快速分离分析。

关键词: 反相液相色谱 , 硅烷偶联剂, 酯型十八烷基键合硅胶整体柱

Abstract: An ester-bonded monolithic silica column for reversed-phase high performance liquid chromatography was synthesized by reacting stearic acid with γ-glycidoxypropyltrimethoxysilane and coupling the intermediate product onto monolithic silica column. Characterization of the prepared column was carried out with Fourier transformation infrared spectrometry and elemental analysis. The chromatographic properties of the packing were evaluated by using benzene, biphenyl, and anthracene as samples and methanol-water as binary mobile phase. The column back-pressure and separation effect were also evaluated for fast separation. The results show that the stationary phase has satisfactory chromatographic properties and resists hydrolysis between pH=2-8, and it can be used for the fast-separation of solutes efficiently.
Key words: silane coupling agent; octadecyl ester-bonded monolithic silica column; reversed-phase liquid chromatographyAntibodies as Tailor-Made Chiral Selectors: an Interdisciplinary
Approach to Enantiomer Separation and DetectionHOFSTETTER Heike, HOFSTETTER Oliver
(Department of Chemistry and Biochemistry, Northern Illinois University, DeKalb, Illinois 60115, USA)Abstract: It has long been known that the configurational isomers of biologically active compounds, e.g., nutrients, pesticides, and drugs, may exhibit different activities in a chiral environment such as the human body. Although the majority of drugs presently in development are chiral, analytical and preparative methods for the quantitative determination and purification of stereoisomers still lag behind. One reason is that commonly used chiral selectors for the direct resolution of enantiomers are not tailor-made for a specific analyte. The identification of suitable selectors for a particular pair of enantiomers still requires considerable experimentation and is generally demanding with regard to material, time and labor. The rational design of chiral host molecules, therefore, represents a challenge in facilitating enantiomer analysis. In this article, we describe how a combination of techniques ranging from organic synthesis to molecular biology yields antibodies of predetermined specificity and stereoselectivity that can be used as tailor-made chiral selectors for the chromatographic separation of enantiomers and their sensitive detection in immunosensors.

Key words: chromatography, immunosensor, stereoselective antibodies , chiral separation