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<p>Mesoporous silica particles were synthesized via investigating polymerization-induced colloidal aggregation (PICA) reaction process in our laboratory. Mesoporous microspheres with a particle size of about 2~7&#xa0;μm and various surface morphology were first compared via varying the pH and molar ratio of formaldehyde/urea in the PICA process. The effects of salts and surfactant on the preparation were further investigated by fixing pH and molar ratio formaldehyde/urea (1:1.5), demonstrated that the particle size distribution became narrower when potassium sulphate and a nonionic surfactant were added together. The morphology, pore size distribution and the specific surface area of the synthesized mesoporous SiO<sub>2</sub> microspheres were observed and characterized by optical microscope, scanning electron microscope (SEM), dynamic light scattering (DLS), and specific surface area (BET) analysis. In the present study, synthesized materials modified octadecyltrichlorosilane (PICA-3@C18) were slurry-packed into a chromatographic empty column, resulting in successful separation of nonpolar compounds. Furthermore, the synthesized materials were functionalized with aminopropyl trimethoxysilane under optimized conditions and exhibited outstanding separation abilities. Aminopropyl trimethoxysilane was further bonded onto commercial SiO<sub>2</sub>, resulting in a stationary phase that exhibited better chromatographic performance than commercial amide columns, NH<sub>2</sub> columns, and other HILIC columns. This work provides insight into retention behavior in HILIC mode and offers a foundation for the development of other amine-based HILIC stationary phases.</p>

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Simply Preparation of Monodisperse SiO2 with the Effects of Inorganic Salts, Surfactants and their Assessment in Liquid Chromatography Applications

  • 期刊论文

  • 发表日期：

    2026年2月24日

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  • Xingyun Zhao,
  • Xiaojian Liu,
  • Zhenwei Zhang,
  • Jiangyan Jin,
  • Siyu Yang,
  • Chengxiao Zhao,
  • Rongfang Wu,
  • Liyun Zhang

摘要

Mesoporous silica particles were synthesized via investigating polymerization-induced colloidal aggregation (PICA) reaction process in our laboratory. Mesoporous microspheres with a particle size of about 2~7 μm and various surface morphology were first compared via varying the pH and molar ratio of formaldehyde/urea in the PICA process. The effects of salts and surfactant on the preparation were further investigated by fixing pH and molar ratio formaldehyde/urea (1:1.5), demonstrated that the particle size distribution became narrower when potassium sulphate and a nonionic surfactant were added together. The morphology, pore size distribution and the specific surface area of the synthesized mesoporous SiO2 microspheres were observed and characterized by optical microscope, scanning electron microscope (SEM), dynamic light scattering (DLS), and specific surface area (BET) analysis. In the present study, synthesized materials modified octadecyltrichlorosilane (PICA-3@C18) were slurry-packed into a chromatographic empty column, resulting in successful separation of nonpolar compounds. Furthermore, the synthesized materials were functionalized with aminopropyl trimethoxysilane under optimized conditions and exhibited outstanding separation abilities. Aminopropyl trimethoxysilane was further bonded onto commercial SiO2, resulting in a stationary phase that exhibited better chromatographic performance than commercial amide columns, NH2 columns, and other HILIC columns. This work provides insight into retention behavior in HILIC mode and offers a foundation for the development of other amine-based HILIC stationary phases.