分會(huì)

第二十七分會(huì)：色譜分離分析

摘要

本文通過三辛基膦與烯丙基溴反應(yīng)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(diǎn)擊化學(xué)”反應(yīng)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(duì)Sil-[P888Allyl]Br固定相材料進(jìn)行表征，顯示該固定相已成功制備。通過對(duì)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(jī)制。利用核苷堿基、磺胺、酰胺、硫脲、苯胺等測(cè)試物，對(duì)所制備固定相的色譜性能進(jìn)行評(píng)價(jià)，五類測(cè)試物均具有較好的分離選擇性和良好的峰對(duì)稱性，最高柱效可達(dá)11萬。進(jìn)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(duì)大豆卵磷脂和胃癌細(xì)胞提取的膜脂均顯示出良好的分離能力，具有良好的應(yīng)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(xué)、陳蕊 中國農(nóng)業(yè)科學(xué)院蜜蜂研究所 共2人點(diǎn)贊了這篇線上墻報(bào)。