应用化学 ›› 2010, Vol. 27 ›› Issue (12): 1457-1461.DOI: 10.3724/SP.J.1095.2010.00056

• 研究论文 • 上一篇    下一篇

甲基丙基酸丁酯/SiO2/TiO2有机-无机杂化毛细管整体柱的制备及应用

李英杰,郝秀菊*,张春雨,梁辉   

  1. (齐齐哈尔大学化学与化学工程学院 齐齐哈尔 161006)
  • 收稿日期:2010-01-25 修回日期:2010-05-10 出版日期:2010-12-10 发布日期:2010-12-10
  • 通讯作者: 李英杰,男,教授; E-mail:lyj310@163.com; 研究方向:电色谱分析

Preparation and Application of the Poly-methyl-propyl-butyl acrylate/SiO2/TiO2 Organic-inorganic Hybrid Capillary Monolithic Column

LI Ying-Jie, HAO Xiu-Ju*, ZHANG Chun-Yu, LIANG Hui   

  1. (Qiqihar University of Chemistry and Chemical Engineering Institute,Qiqihar 161006)
  • Received:2010-01-25 Revised:2010-05-10 Published:2010-12-10 Online:2010-12-10

摘要:

采用溶胶-凝胶法制备了SiO2/TiO2杂化材料,并通过双官能团试剂3-(甲氧基硅烷基)甲基丙烯酸丙酯(γ-MAPS)对其进行改性;改性溶胶与甲基丙基酸丁酯(BMA)作为功能单体,在毛细管中进行原位聚合反应,制备了新型的有机-无机杂化毛细管整体柱。 采用扫描电子显微镜观察了整体柱柱床的形貌。 以硫脲为电渗流标记物对所制备的整体柱进行了柱性能评价,考察了柱的稳定性和重现性,获得了88000 plates/m的柱效;考察了中性物质在柱上的的保留行为,得出该柱具有反相电色谱保留性能。 通过对2种短肽(磷酸肽和非磷酸肽)洗脱测试,实现了对磷酸肽的有效富集与分离。

关键词: 整体柱, 毛细管电色谱, 溶胶-凝胶法, 有机-无机杂化材料, 磷酸肽

Abstract:

SiO2/TiO2 hybrid materials were prepared via a sol-gel process followed with modification by bifunctional reagent of 3-(methoxy-silane-yl) propyl methacrylate(γ-MAPS). A new type of organic-inorganic hybrid capillary monolithic column was prepared in the capillary tube by in-situ polymerization of modified SiO2/TiO2 sol and poly-methyl-propyl-butyl acrylate(BMA). The microstructures of the bed-column cross-section were characterized by scanning electron microscopy(SEM). The column efficiency of 88000 plates per meter was obtained on the basis of evaluating the performance of the as-prepared monolithic column using thiourea as the electroosmotic flow(EOF) marker and investigating the stability and reproducibility of the column as well as the retention behavior of the neutral material on the column. The phosphorpeptide′s effective enrichment and separation were realized by the elution test of two kinds of short peptides(phosphoric acid peptide and non-phosphorylated peptides).

Key words: monolithic columns, capillary electrochromatography, sol-gel method, organic-inorganic hybrid materials, phosphopeptides

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