In-situ growth of a spherical vinyl-functionalized covalent organic framework as stationary phase for capillary electrochromatography-mass spectrometry analysis.

Column technology is an important part in capillary electrochromatographic science. Developing novel stationary phase with high separation efficiency and high loading capacity is an essential work. In this work, a novel spherical vinyl-functionalized covalent-organic framework (COF-V) was synthesized at room temperature and firstly employed as stationary phase for CEC-MS analysis. The COF-V based CEC column was characterized by scanning electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The results proved the successful modification of COF-V. The COF-V based column possesses the advantages like strong electroosmotic flow, high separation efficiency and high loading capacity. The CEC column showed powerful separation selectivity to several kinds of compounds, and the highest column efficiency (theoretical plates, N) was over 1.4 × 105 plates·m-1 for methylbenzene. Besides, the COF-V modified column exhibited excellent repeatability and stability. The relative standard deviations (RSDs) of retention times for intra-day (n = 5), inter-day (n = 3) runs and column-to-column (n = 3) were all less than 2.1%. Hence, the COF-V modified column was successfully applied in CEC-MS for determination of antiepileptic drug, triazine herbicides and active ingredients in traditional Chinese medicine.