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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
引用本文:王利娟,杨更亮,李煦,李晓瑜,尹俊发,李志伟,高文惠,杨静,陈义.酯型十八烷基键合硅胶整体柱的制备、表征及性能评价[J].色谱,2005,23(5):504-507.
作者姓名:王利娟  杨更亮  李煦  李晓瑜  尹俊发  李志伟  高文惠  杨静  陈义
作者单位: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
基金项目:国家自然科学基金资助项目(No.20375010)、教育部高等学校博士学科点专项科研基金项目、教育部优秀青年教师资助计划项目、中国科学院“百人计划”项目.
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  
文章编号:1000-8713(2005)05-0504-04
收稿时间:2005-05-19
修稿时间:2005年5月19日

Synthesis, Characterization and Evaluation of Octadecyl Ester-Bonded Monolithic Column
WANG Lijuan,YANG Gengliang,LI Xu,LI Xiaoyu,YIN Junfa,LI Zhiwei,GAO Wenhui,YANG Jing,CHEN Yi.Synthesis, Characterization and Evaluation of Octadecyl Ester-Bonded Monolithic Column[J].Chinese Journal of Chromatography,2005,23(5):504-507.
Authors:WANG Lijuan  YANG Gengliang  LI Xu  LI Xiaoyu  YIN Junfa  LI Zhiwei  GAO Wenhui  YANG Jing  CHEN Yi
Institution: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
Abstract:An ester-bonded monolithic silica column for reversed-phase high performance liquid chromatography was synthesized by reacting stearic acid with y-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.
Keywords:silane coupling agent  octadecyl ester-bonded monolithic silica column  reversed-phase liquid chromatography
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