分会

第二十七分会：色谱分离分析

摘要

本文通过三辛基膦与烯丙基溴反应制备了一种新型季膦离子液体三辛基（烯丙基）溴化磷，将新型季膦离子液体通过一步法“点击化学”反应键合到巯基功能化的硅胶表面，制备了新型聚合季膦离子液体修饰固定相（Sil-[P888Allyl]Br）。首先利用傅里叶变换红外光谱仪，热重分析仪和元素分析对Sil-[P888Allyl]Br固定相材料进行表征，显示该固定相已成功制备。通过对烷基苯和核苷碱基保留特性的研究，显示Sil-[P888Allyl]Br填充柱具有亲水/疏水混合模式保留机制。利用核苷碱基、磺胺、酰胺、硫脲、苯胺等测试物，对所制备固定相的色谱性能进行评价，五类测试物均具有较好的分离选择性和良好的峰对称性，最高柱效可达11万。进一步将Sil-[P888Allyl]Br填充柱用于磷脂酰胆碱亚类和磷脂混合物的分离，结果表明具有良好的分离选择性。此外，Sil-[P888Allyl]Br固定相对大豆卵磷脂和胃癌细胞提取的膜脂均显示出良好的分离能力，具有良好的应用潜能。 Herein, phosphonium-based ionic liquid trioctyl(allyl) phosphonium bromide was firstly prepared by the reaction of trioctylphosphine and allyl bromide. The synthesized ionic liquid was further used to graft sulfhydryl-functionalized silica and the new polymerized phosphonium ionic liquid-based stationary phase ([P888Allyl]Br) can be successfully obtained. The Sil-[P888Allyl]Br stationary phase material was characterized by FT-IR, thermogravimetric analysis and elemental analysis. The result demonstrates the new stationary phase was successfully fabricated. The developed Sil-[P888Allyl]Br stationary phase indicates hydrophilic/hydrophobic mixed-mode retention mechanism and the packed column was successfully used to separate of nucleoside bases, sulfonamides, amides, thioureas and anilines. The maximum column efficiency can reach 110,000 plates/m. The Sil-[P888Allyl]Br column was also successfully used to separate phosphatidylcholine mixture as well as different kinds of phospholipid mixtures.

关键词

季膦离子液体;混合模式固定相;高效分离;磷脂

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刘德禄 河北大学、陈蕊 中国农业科学院蜜蜂研究所 共2人点赞了这篇线上墙报。