分會

第二十七分會：色譜分離分析

摘要

本文通過三辛基膦與烯丙基溴反應制備了一種新型季膦離子液體三辛基（烯丙基）溴化磷，將新型季膦離子液體通過一步法“點擊化學”反應鍵合到巰基功能化的硅膠表面，制備了新型聚合季膦離子液體修飾固定相（Sil-[P888Allyl]Br）。首先利用傅里葉變換紅外光譜儀，熱重分析儀和元素分析對Sil-[P888Allyl]Br固定相材料進行表征，顯示該固定相已成功制備。通過對烷基苯和核苷堿基保留特性的研究，顯示Sil-[P888Allyl]Br填充柱具有親水/疏水混合模式保留機制。利用核苷堿基、磺胺、酰胺、硫脲、苯胺等測試物，對所制備固定相的色譜性能進行評價，五類測試物均具有較好的分離選擇性和良好的峰對稱性，最高柱效可達11萬。進一步將Sil-[P888Allyl]Br填充柱用于磷脂酰膽堿亞類和磷脂混合物的分離，結(jié)果表明具有良好的分離選擇性。此外，Sil-[P888Allyl]Br固定相對大豆卵磷脂和胃癌細胞提取的膜脂均顯示出良好的分離能力，具有良好的應用潛能。 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.

關(guān)鍵詞

季膦離子液體;混合模式固定相;高效分離;磷脂

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劉德祿 河北大學、陳蕊 中國農(nóng)業(yè)科學院蜜蜂研究所 共2人點贊了這篇線上墻報。