Synthesis of monodisperse silica microspheres and modification with diazoresin for mixed‐mode ultra high performance liquid chromatography separations

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EarlyView Article

  • Published: Oct 4, 2017
  • Author: Hailin Cong, Bing Yu, Chao Tian, Shuai Zhang, Hua Yuan
  • Journal: Journal of Separation Science


Monodisperse silica particles with average diameters of 1.9–2.9 μm were synthesized by a modified Stöber method, in which tetraethyl orthosilicate was continuously supplied to the reaction mixture containing KCl electrolyte, water, ethanol, and ammonia. The obtained silica particles were modified by self‐assembly with positively charged photosensitive diazoresin on the surface. After treatment with ultraviolet light, the ionic bonding between silica and diazoresin was converted into covalent bonding through a unique photochemistry reaction of diazoresin. Depending on the chemical structure of diazoresin and mobile phase composition, the diazoresin‐modified silica stationary phase showed different separation mechanisms, including reversed phase and hydrophilic interactions. Therefore, a variety of baseline separation of benzene analogues and organic acids was achieved by using the diazoresin‐modified silica particles as packing materials in ultra high performance liquid chromatography. According to the π–π interactional difference between carbon rings of fullerenes and benzene rings of diazoresin, C60 and C70 were also well separated by ultra‐high performance liquid chromatography. Because it has a small size, the ∼2.5 μm monodisperse diazoresin‐modified silica stationary phase shows ultra‐high efficiency compared with the commercial C18‐silica high‐performance liquid chromatography stationary phase with average diameters of ∼5 μm.

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