厚朴酚键合硅胶液相色谱固定相的制备、表征与性能评价  

Preparation,Characterization and Evaluation of Magnolol-bonded Silica Gel Stationary Phase for Reversed-phase Liquid Chromatography

作　　者：李来生[1] 陈红[1] 马海萍[1] 方奕珊[1] 

机构地区：[1]南昌大学分析测试中心,南昌330047

出　　处：《高等学校化学学报》2012年第4期707-713,共7页Chemical Journal of Chinese Universities

基　　金：国家自然科学基金(批准号:21165012);江西省自然科学基金(批准号:2010GZH0089);江西省教育厅科技项目(批准号:GJJ11274)资助

摘　　要：通过γ-巯丙基三甲氧基硅烷(KH-590)的作用,将具有抗菌功能的中草药厚朴的主要药用成分厚朴酚键合在硅胶表面上,制备了厚朴酚键合硅胶液相色谱固定相.采用红外光谱、元素分析和热重分析对该固定相进行了表征.以苯同系物、5种吡啶、6种苯胺和8种芳香羧酸类化合物为溶质探针,初步考察了该新型固定相的基本色谱性能,研究了其对这些化合物的保留机理.结果表明,该固定相的反相色谱性能类似于十八烷基键合硅胶固定相(ODS),分离原理与疏水性作用有关;另外,该固定相包含有别于疏水性作用的氢键作用、π-π电荷转移作用和偶极-偶极等作用,多种作用力使其在分离某些可电离的碱性和酸性化合物时表现出更好的选择性和分离效果.厚朴酚配体的多种作用位点对快速分离极性芳香化合物有重要贡献.Cortex magnoliae officianalis is a Chinese herbal medicine,which has anti-bacterial function.Magnolol is the main pharmacological component.A new magnolol-bonded silica gel stationary phase（MSP） for reversed-phase liquid chromatography was prepared using 3-mercaptopropyl trimethoxysilane（KH-590） as the coupling reagent.The chemical structure of MSP was characterized by Fourier transform infrared spectroscopy（FTIR）,elemental analysis（ES） and thermogravimetric analysis（TGA）.With the purpose of evaluating the chromatographic performance and elucidating the related retention mechanism on the new packing material,some alkylbenzene homologues,five pyridines,six aniline compounds and eight aromatic carboxylic acids were used as neutral,basic and acidic probes,respectively.The results showed that MSP could be considered as a reversed-phase liquid chromatographic stationary phase,which was similar to ODS column.The principle of the chromatographic separation for most analytes on MSP column involved hydrophobic interaction.Moreover,MSP is a packing material that has versatile chromatographic functions.The chromatographic results indicated that hydrophobic interaction,hydrogen bonding interaction,π-π interaction and dipole-dipole interaction between the bonded phase and analytes play significant roles in the retention of some basic compounds and aromatic carboxylic acids,and better selectivity and separation have been presented on MSP column.Various action sites of mognolol could contribute to the fast separations of many polar aromatic compounds.

关 键 词：高效液相色谱 键合硅胶固定相 厚朴酚 色谱性能 碱性化合物 

分 类 号：O657[理学—分析化学]