色谱Issue(8)：798-803,6.DOI:10.3724/SP.J.1123.2014.04038
大黄素键合硅胶高效液相色谱柱的制备和应用
Preparation and application of an emodin-bonded silica gel chromatographic column for high performance liquid chromatography
摘要
Abstract
An emodin-bonded silica gel stationary phase( ESP)for high performance liquid chromatography has been synthesized by the intermediate method. The preparation process was as follows:γ-glycidoxypropyltrimethoxy silane( KH-560)firstly reacted with emodin ligand;then the intermediate was chemically immobilized to the surface of silica gel. Characterization of ESP was carried out with Fourier transform infrared spectroscopy ( FTIR ), elemental analysis and thermogravimetric analysis. Naphthalene was used as a probe to determine the col-umn efficiency with methanol-water(60 :40,v / v)as binary mobile phase at a flow rate of 0. 8 mL / min. In order to elucidate the related separation mechanism,ESP was used to separate a series of neutral,basic and acidic aromatic compounds,as well as a sample of wind medicated oil. The conventional C 18 column and phenyl column were also tested under the same chromato-graphic conditions for comparison. The results showed that the emodin ligand was successfully bonded to the surface of spherical silica gel with a 0. 23 mmol / g of bonded amount,and the theoretical plate number of ESP column was about 19 874 N / m. The coupling reagent chains and anthraquinone rings in ESP offered a structural basis for hydrophobic interaction. Mean-while,the emodin ligands provided π-π or p-π,charge transfer,hydrogen bonding,dipole-di-pole action sites for different analytes. The synergistic reaction of various action sites endowed ESP column special and excellent chromatographic separation selectivity. And a baseline sepa-ration of polar compounds such as amines and phenols on ESP was easily achieved by using common and cheap methanol-water mobile phases without buffer salts. The experimental condi-tions were simple and convenient.关键词
高效液相色谱/键合硅胶固定相/大黄素配体/色谱柱/制备/应用Key words
high performance liquid chromatography( HPLC)/bonded silica gel stationary phase/emodin ligand/chromatographic column/preparation/application分类
化学化工引用本文复制引用
许丽丽,任乃林,林泽玲..大黄素键合硅胶高效液相色谱柱的制备和应用[J].色谱,2014,(8):798-803,6.基金项目
韩山师范学院青年项目（ LQ200906）；潮州市科技引导计划项目（2013H04）． （）
