High stability amino-derived reversed-phase/anion-exchange mixed-mode phase based on polysilsesquioxane microspheres...

A series of amino-derived mixed-mode chromatographic stationary phases were synthesized based on porous mercaptopropyl-functionalized polysilsesquioxane mesoporous microspheres synthesized by a co-condensation of methyltrimethoxysilane (MTMS) and mercaptopropyltrimethoxysilane (MPTMS). Through controlling the ratio of MTMS and MPTMS, the modified stationary phases with different amino densities were prepared by a "thiol-ene" click chemistry reaction. The morphology, pore structure, and functional groups of the microspheres were characterized by scanning electron microscope (SEM), nitrogen adsorption-desorption test, Fourier transform infrared spectroscopy (FT-IR), elemental analysis, and zeta potential, respectively. The chromatographic behavior of the stationary phases was evaluated by using alkylbenzene homologs and inorganic anions as probes. The mixed-mode retention behavior and separation mechanisms for neutral, alkaline, and acidic drugs on the prepared column had been systematically studied by changing the value of pH, ionic, and solvent strength of the mobile phase. Compared with the silica-based amino-bonded column (S-NH₂), the synthesized organosilica phase exhibited higher hydrothermal stability and longer service life under high alkaline conditions. The newly synthesized phase was successfully applied to the simultaneous separation of the multiple substances in compound drugs.