title: Facile preparation of organic-silica hybrid monolith for capillary hydrophilic liquid chromatography based on "thiol-ene" click chemistry.
abstract: 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 ζ-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.
authors: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
authors: Ming-Luan
authors: ML
authors: Chen
authors: Jun
authors: J
authors: Zhang
authors: Zheng
authors: Z
authors: Zhang
authors: Bi-Feng
authors: BF
authors: Yuan
authors: Qiong-Wei
authors: QW
authors: Yu
authors: Yu-Qi
authors: YQ
authors: Feng
mesh_terms: D000227:Adenine Nucleotides / Q000737:chemistry / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000295:instrumentation*; D057930:Click Chemistry / Q000379:methods*; D057927:Hydrophobic and Hydrophilic Interactions; D009705:Nucleosides / Q000737:chemistry / Q000302:isolation & purification; D012821:Silanes / Q000138:chemical synthesis / Q000737:chemistry*
chemical_list: D000227:Adenine Nucleotides; D009705:Nucleosides; D012821:Silanes