Synthesis of spherical three-dimensional covalent organic frameworks and in-situ preparation of capillaries coated with them for capillary electrochromatographic separation.

Covalent organic frameworks (COFs) are divided into two-dimensional (2D) and three-dimensional (3D) structures according to the connection dimension of covalent bonds. 3D COFs have smaller pore size and larger surface area, which would facilitate the separation of small organic molecules with similar structures and properties in capillary electrochromatographic (CEC) separation. However, the application of 3D COFs in CEC is still in its early stages. Thus, 3D COFs (3D-IL-COF-1 and 3D-IL-COF-2) were synthesis by a new synthesis method in this work. The related characterization results confirmed that spherical 3D-IL-COFs formed by the accumulation of small polyhedral particles were successfully synthesized. Then, 3D-IL-COFs were introduced into the inner wall of capillary by in-situ growth method to prepare the 3D COFs coated capillaries for the first time. The electrochromatographic separation performance of the 3D-IL-COFs coated capillaries was investigated using the 3D-IL-COF-1 coated capillary as the model. The results indicate that the 3D-IL-COF-1 coated capillary with uniform coating exhibits a broad-spectrum separation capacity not only for acidic, basic and neutral analytes but also for neutral isomers, which shows that 3D-IL-COFs becomes an attractive potential stationary phase for electrochromatographic separation.