双齿键合叔胺/磺酸甜菜碱共修饰亲水硅胶色谱固定相的制备与应用OA

In this study,a tertiary amine silane coupling agent bearing bis[3-(trimethoxysilyl)pro‑pyl]groups was first synthesized via the nucleophilic ring-opening reaction of N,N'-dimethyl-1,3-propanediamine with KH560(γ-glycidoxypropyltrimethoxysilane),which was then grafted onto the surface of silica gel.Subsequently,the silane coupling agent-bonded silica microspheres were fur‑ther reacted with 1,3-propanesultone to afford a bidentate-bonded silica chromatographic stationary phase(denoted as Sil-SAI).Fourier transform infrared spectroscopy(FT-IR)and elemental analysis(EA)confirmed that the Sil-SAI stationary phase was successfully modified with sulfobetaine zwitter‑ionic and tertiary amine bifunctional groups.Furthermore,the separation mechanism of the Sil-SAI column,the effects of buffer salt concentration and pH value of the mobile phase on chromatographic retention behavior,as well as the hydrolytic stability of the stationary phase were systematically in‑vestigated.The results indicated that:Sil-SAI exhibits a typical hydrophilic interaction liquid chro‑matography(HILIC)separation mechanism.Owing to the multiple interactions(including hydrophilic interaction,electrostatic interaction,hydrogen bonding,and dipole-dipole interactions)between probe molecules and the Sil-SAI stationary phase,this stationary phase presents a mixed separation mechanism involving both partition and adsorption processes;With variations in the concentration and pH of the buffer salt in the mobile phase,the neutral,acidic,and basic probe molecules dis‑play distinct chromatographic retention behaviors;Benefiting from its bidentate bonding structure,the Sil-SAI stationary phase possesses superior hydrolytic stability.The application of Sil-SAI station‑ary phase for the separation of six sugars and seven sugar alcohols demonstrated excellent separation efficiency and satisfactory separation reproducibility for all analytes.