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

作　　者：许丽丽[1] 任乃林[1] 林泽玲[1] 

机构地区：[1]韩山师范学院化学系,广东潮州521041

出　　处：《色谱》2014年第8期798-803,共6页Chinese Journal of Chromatography

基　　金：韩山师范学院青年项目(LQ200906);潮州市科技引导计划项目(2013H04)

摘　　要：采用中间体法,先将大黄素配体与γ-[(2,3)-环氧丙氧]丙基三甲氧基硅烷(KH-560)偶联剂反应制备含配体的硅氧烷试剂,然后再与硅胶键合,最终制得大黄素键合硅胶液相色谱固定相(以下简称ESP)。通过红外光谱、元素分析和热重分析表征固定相的结构。以萘作为溶质探针,甲醇-水(60∶40,v/v)为流动相,流速为0.8 mL/min,测得ESP柱的柱效。采用传统的反相C18和苯基柱作参比,将ESP应用于系列中性、碱性和酸性芳香族化合物以及实际样品风油精的分离分析,并探讨相关的色谱分离机理。结果表明,配体大黄素被成功地键合到球形硅胶表面,测得配体键合量为0.23 mmol/g,ESP柱理论塔板数约为19874 N/m。ESP的偶联剂链和蒽醌环提供了疏水性的结构基础,大黄素配体还能为溶质提供π-π或p-π、电荷转移、氢键、偶极-偶极等作用点。多位点的协同作用使得ESP柱具有独特和优秀的色谱分离选择性,并且无需调节pH值,采用简单而廉价的甲醇-水流动相就能实现胺类、酚类等极性样品的基线分离,实验条件简单、方便。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 

分 类 号：O658[理学—分析化学]