Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1284, Issue -, Pages 118-125Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2013.02.008
Keywords
Organic-silica hybrid monolith; Thiol-ene click chemistry; Capillary liquid chromatography; Hydrophilic interaction chromatography
Funding
- National Nature Science Foundation of China [91217309, 91017013, 31070327]
- National Basic Research Program of China (973 Program) [2012CB720601, 2013CB910700]
- Fundamental Research Funds for the Central Universities
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In this work, a one-step approach to facile preparation of organic-inorganic hybrid monoliths was successfully developed. After vinyl-end organic monomers and azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethoxysilane (TMOS) and 3-mercaptopropyltrimethoxysilane (MPTMS), the homogeneous mixture was introduced into a fused-silica capillary for simultaneous polycondensation and thiol-ene click reaction to form the organic-silica hybrid monoliths. By employing this strategy, two types of organic-silica hybrid monoliths with positively charged quaternary ammonium and amide groups were prepared, respectively. The functional groups were successfully introduced onto the monoliths during the sol-gel process with thiol-ene click reaction, which was demonstrated by zeta-potential assessment, energy dispersive X-ray spectroscopy (EDX), and Fourier transform infrared (FT-IR) spectroscopy. The porous structure of the prepared monolithic columns was examined by scanning electron microscopy (SEM), nitrogen adsorption-desorption measurement, and mercury intrusion porosimetry. These results indicate the prepared organic-silica hybrid monoliths possess homogeneous column bed, large specific surface area, good mechanical stability, and excellent permeability. The prepared monolithic columns were then applied for anion-exchange/hydrophilic interaction liquid chromatography. Different types of analytes, including benzoic acids, inorganic ions, nucleosides, and nucleotides, were well separated with high column efficiency around 80,000-130,000 plates/m. Taken together, we present a facile and universal strategy to prepare organic-silica hybrid monoliths with a variety of organic monomers using one-step approach. (C) 2013 Elsevier B.V. All rights reserved.
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