纳米氧化锆沉积硅胶色谱固定相的制备及亲水作用色谱行为  

Preparation of Zirconia Deposited Silica Stationary Phase and Its Application to Hydrophilic-interaction Liquid Chromatography

作　　者：余琼卫[1] 郑凤 方凯敏 冯钰锜[1] YU Qiongwei;ZHENG Feng;FANG Kaimin;FENG Yuqi(Key Laboratory of Analytical Chemistry for Biology and Medicine,Ministry of Education, College of Chemistry and Molecular Sciences,Wuhan University,Wuhan 430072,China)

机构地区：[1]生物医学分析化学教育部重点实验室武汉大学化学与分子科学学院

出　　处：《高等学校化学学报》2019年第9期1857-1865,共9页Chemical Journal of Chinese Universities

基　　金：国家自然科学基金(批准号:31671929,31670373)资助~~

摘　　要：采用液相沉积法(LPD)制备了纳米氧化锆沉积硅胶色谱固定相(ZrO2/SiO2),并将其应用于亲水作用色谱分离中.考察并比较了ZrO2/SiO2、硅胶(SiO2)和氧化锆(ZrO2) 3种色谱固定相在不同有机调节剂比例、不同pH值及不同盐浓度的流动相条件下的色谱行为.结果表明,制备的ZrO2/SiO2色谱柱不仅具有SiO2色谱柱高柱效的优点,表面沉积的纳米氧化锆还能有效屏蔽硅羟基,有利于碱性物质的保留和分离,表现出良好的亲水作用色谱性能.将ZrO2/SiO2色谱柱用于4种脱氧核苷和5种碱性化合物的分离,均得到了较好的效果,展现出其作为色谱固定相良好的应用前景.ZrO 2 nanoparticles were deposited on silica by LPD method and the resulting ZrO 2/SiO 2 was employed as stationary phase in hydrophilic-interaction liquid chromatography. The chromatographic perfor-mance of three columns packed with SiO 2, ZrO 2/SiO 2 and ZrO 2 were compared. The results showed that the column packed with ZrO 2/SiO 2 not only had the advantages of high column efficiency like the SiO 2 column, but also the deposited zirconia nanoparticles on the silica surface could shield the silicon hydroxyl group effectively, which benefit for the retention and separation of alkaline substances and showed good hydrophilic-interaction chromatographic performance. Effective separation of 4 deoxynucleosides and 5 basic compounds was achieved on ZrO 2/SiO 2 column in the hydrophilic-interaction liquid chromatography(HILIC) mode.

关 键 词：液相沉积法 氧化锆 亲水作用色谱 保留机理 

分 类 号：O657[理学—分析化学]