溴化1-乙烯基-3-十二烷基咪唑硅胶键合固定相制备及其色谱性能  

Preparation and chromatographic properties of 1-vinyl-3-dodecylimidazole bromide silica-bonded stationary phase

作　　者：李新庭 梁鹏 周玉凤 乔晓强[1] LI Xinting;LIANG Peng;ZHOU Yufeng;QIAO Xiaoqiang(College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China)

机构地区：[1]河北大学药学院,河北保定071002

出　　处：《色谱》2020年第11期1263-1269,共7页Chinese Journal of Chromatography

基　　金：河北省杰出青年科学基金(B2019201327);河北省高校百名优秀创新人才项目(SLRC2019016).

摘　　要：膜脂作为细胞质膜的主要组成部分,在生命活动中扮演着重要的作用,其涉及多种重要疾病的发生和发展过程。发展适用于膜脂分离分析的新型色谱材料对于其后续结构和生物学功能研究具有重要的意义。该文选用具有潜在生物相容性的离子液体溴化1-乙烯基-3-十二烷基咪唑(1-vinyl-3-dodecylimidazole bromide,VDI)为功能单体,通过一步法点击反应将其接枝到巯基功能化硅球表面,制备得到了新型溴化1-乙烯基-3-十二烷基咪唑硅胶键合固定相(Sil-VDI)。利用傅里叶变换红外光谱仪和热重分析仪对Sil-VDI固定相材料的结构进行表征,结果证明Sil-VDI色谱固定相已被成功制备。保留机制研究显示填充Sil-VDI色谱柱具有典型的反相/离子交换混合模式保留特性。基于此,采用不同疏水性物质烷基苯、多环芳烃、苯胺、苯衍生物和无机阴离子BrO-3、NO-3和IO-3为测试物,对所制备固定相的色谱性能进行了研究。结果表明,该固定相对4类疏水性物质和无机阴离子均有较好的分离选择性和良好的峰对称性。进一步研究了所制备的Sil-VDI色谱柱对鸡蛋黄磷脂和肺腺癌细胞提取膜脂的分离效果,结果显示Sil-VDI色谱柱对2种磷脂样品均显示出了良好的分离能力。该文所制备的Sil-VDI色谱固定相合成方法简便,具有良好的分离分析应用潜能,后续工作会进一步研究该固定相在生物样品中的分离分析性能。As the main components of cell membranes,lipids play important roles in organisms.Lipids have been proved to be closely associated with the occurrence and development of serious diseases,such as cancers and metabolic diseases.The development of novel separation materials for use in high-performance liquid chromatography(HPLC)is essential for high-efficiency lipid separation.Such materials can promote further in-depth research of the structure and biological functions of lipids.In this study,we focused on the preparation of an ionic-liquid-modified silica-bonded HPLC stationary phase and on its chromatographic retention mechanisms and separation performances for lipids.An imidazolium-based ionic liquid with C12 side chain,viz.1-vinyl-3-dodecylimidazole bromide(VDI),has shown good biocompatibility and has previously been used for the solubilization of membrane proteins.Thus,VDI was first exploited as the functionalized monomer for the HPLC stationary phase.It was grafted onto the surface of thiol-functionalized silica spheres by a one-step click reaction to afford a new VDI silica-bonded stationary phase(Sil-VDI).Fourier-transform infrared(FT-IR)spectroscopy and thermogravimetric analysis were used to prove the successful preparation of Sil-VDI and characterize its structure.The chromatographic retention properties of the column packed with Sil-VDI was first studied using hydrophobic alkylbenzenes.The results showed that the Sil-VDI column was a typical reversed-phase liquid chromatography retention column.Since Sil-VDI has a permanent cationic imidazole structure,it should demonstrate anion exchange retention.Thus,inorganic anions BrO-3,NO-3,and IO-3 were selected to further investigate the retention mechanism of the Sil-VDI column.The results demonstrate that the Sil-VDI column also possesses ion-exchange retention mode.Thus,the Sil-VDI column has typical reversed-phase and ion-exchange mixed-mode retention characteristics.Based on the reversed-phase retention characteristics of the Sil-VDI column,hydrophobic alk

关 键 词：离子液体 键合固定相 反相/离子交换色谱 膜脂分离 

分 类 号：O658[理学—分析化学]