One-pot Facile Preparation of Amino-functionalized Silica Hybrid Monoliths for Mixed-mode Chromatography

  • Firda Furqani Division of Materials Engineering, Graduate School of Engineering, Gifu University, Japan
  • Lee Wah Lim Division of Materials Engineering, Graduate School of Engineering, Gifu University, Japan
  • Toyohide Takeuchi Division of Materials Engineering, Graduate School of Engineering, Gifu University, Japan
Keywords: Amino-functionalized mixed-mode stationary phase, Capillary liquid chromatography, Hybrid monolithic column, Inorganic anions, Nucleosides


Silica hybrid monolithic columns were prepared using two precursors, in which organo-functionalized trialkoxysilanes are mixed with tetraalkoxysilanes. In this study, several types of amino-functionalized silica hybrid monolithic columns were prepared via single-step “one-pot” approach, and the amount of silica precursors, porogens, as well as the reaction conditions were optimized. The preparation was carried out by mixing the silica precursors, i.e. tetraethoxysilane (TEOS) or tetramethoxysilane (TMOS) with amino precursors such as aminopropyltrimethoxysilane (APTES), aminoethylaminopropyl-trimethoxysilane (AEAPTMS), and phenylaminopropyltrimethoxysilane (PAPTMS) in a porogenic solution. The chromatographic performance of these hybrid monolithic columns was optimized by investigating several parameters through the separation of inorganic anions (IO3-, BrO3-, Br-, NO2-, NO3-, I-, SCN-) and some polar compounds (thymine, thymidine, adenosine, adenine, uridine). Results showed that the silica hybrid monolithic columns could be operated at higher flow-rate that favors rapid separation. The run-to-run repeatability of Si-APTES and Si-PAPTMS hybrid monolithic columns were satisfactory with relative standard deviations (n = 5) of less than 8% for all the analyte anions.


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Amino-functionalized silica precursors was used in the preparation of hybrid monolithic column to reduce the preparation time via one-pot approach. The amine groups in the structure can provide weak anion exchange interaction and also hydrophilic interaction. The synthesized hybrid monolithic columns revealed good mechanical stability and good separation repeatability.
How to Cite
Furqani, F., Lim, L. W., & Takeuchi, T. (2019). One-pot Facile Preparation of Amino-functionalized Silica Hybrid Monoliths for Mixed-mode Chromatography. Journal of the Indonesian Chemical Society, 2(2), 81.