高等学校化学学报2024，Vol.45Issue(4)：71-80,10.DOI:10.7503/cjcu20230503
酰胺和咪唑基离子液体双极性基团共嵌入式亲水C18硅胶固定相的制备与应用
Preparation and Application of Imidazole-based Ionic Liquid and Amide Bipolar Groups Co-embedded Hydrophilic C18 Silica Gel Stationary Phase
摘要
Abstract
In this work,octadecyl-modified silica chromatographic stationary phases with amide and imidazole-based ionic liquid bipolar groups co-embedded were prepared by stepwise bonding and two stationary phases with different anionic coordinations(Sil-IL-AMC18-Cl and Sil-IL-AMC18-Tf2N)were prepared by ion-exchange,which were characterized by means of infrared spectroscopy and elemental analysis.Both stationary phases showed C=C stretching vibration peaks and C=N bending vibration peaks on the imidazole ring at 1460 and 661 cm‒1,and asym-metric and symmetric stretching vibration peaks of—CH at 2927 and 2856 cm‒1,which proved the bonding of amino-imidazole ionic liquid.And the original 919 cm‒1 of primary amine N—H out-of-plane deformation vibration peak dis-appeared,indicating that octadecanoyl chloride is bonded with amino.The results of elemental analysis showed that Sil-IL-AMC18-Cl contained 3.07%of nitrogen,16.73%of carbon and 3.07%of hydrogen,and Sil-IL-AMC18-Tf2N contained 2.88%of nitrogen,15.98%of carbon and 2.95%of hydrogen,which indicated that Sil-IL-AMC18-Cl and Sil-IL-AMC18-Tf2N chromatographic stationary phases were prepared.The chromatographic separation modes and performance of Sil-IL-AMC18-Cl and Sil-IL-AMC18-Tf2N stationary phases were investigated,and the results showed that:(1)the two stationary phases had higher column efficiency than commercial C18 columns in the reversed-phase chromatographic mode(RPLC);(2)since the stationary phase has a bipolar group,it has a stronger hydrophilic ability compared to the traditional hydrophilic modified C18 silica stationary phase,and thus hydrophilic chromato-graphic mode(HILIC)can be realized;(3)simultaneous separation of hydrophilic and hydrophobic substances in mixed reversed-phase/hydrophilic(RPLC/HILIC)chromatographic mode.It was found that Sil-IL-AMC18-Cl stationary phase had stronger hydrophilic properties compared to Sil-IL-AMC18-Tf2N stationary phase,so in the HILIC chromatographic mode Sil-IL-AMC18-Cl stationary phase was used for the separation of 8 base nucleosides,which could realize the baseline separation of this kind of strong hydrophilic substances,and the RSD of the injection repeatability was 0.03%—0.25%(n=9);in the RPLC chromatographic mode,Sil-IL-AMC18-Tf2N stationary phase was used for the separation of 6 anilines,which not only could realize the baseline separation,but also improved the peak trailing problem of anilines,and the RSD of the injection repeatability was 0.05%—0.10%(n=9).关键词
亲水改性C18硅胶填料/混合模式液相色谱固定相/碱基核苷/苯胺Key words
Hydrophilic modified C18 silica gel filler/Mixed-mode liquid chromatography stationary phase/Base nucleoside/Aniline分类
化学化工引用本文复制引用
陈贝怡,观文娜,靳钊,刘婷婷,周睿..酰胺和咪唑基离子液体双极性基团共嵌入式亲水C18硅胶固定相的制备与应用[J].高等学校化学学报,2024,45(4):71-80,10.基金项目
中国科学院仪器设备功能开发技术创新项目资助. Supported by the Instrument and Equipment Function Development Technology Innovation Project of Chinese Academy of Sciences. （）
