Since some metal‐organic cages (MOCs) have been synthesized in past several years, the applications of MOCs such as drug delivery, molecular recognition, separation, catalysis, and gas storage, etc. have been witnessed with a significant increase. However, to the best of our knowledge, so far no one has used MOCs as chiral stationary phase to separate chiral compounds in CEC. In this study, three MOCs were developed as the stationary phase for CEC separation of enantiomers. The MOCs coated capillary column showed good chiral recognition ability for some chiral compounds, including amine, alcohols, ketone, etc. The influence of buffer concentration, applied voltage, pH of buffer solution on the chiral separations was also investigated. The RSDs of run‐to‐run, day‐to‐day, and column‐to‐column for retention time were 2.1‐4.67%, 1.2‐4.36%, and 3.62‐6.43%, respectively. This work reveals that the chiral MOCs material is feasible for the enantioseparation in CEC.

Bi-2-naphthol is a kind of commonly used chiral molecule that has been widely applied in the fields of molecular recognition, materials, and asymmetric synthesis. Since there are few examples of utilizing (R)-1,1′-bi-2-naphthol derivatives used as stationary phases to resolve chiral compounds by capillary electrochromatography, three The (R)-1,1′-bi-2-naphthol derivatives were synthesized and used as stationary phases to fabricate capillary columns for chiral separation. Some of the experimental parameters for enantiomer separations were optimized. the columns exhibited good enantioselectivity for chiral alcohols, amines, ketones, and so forth. The relative standard deviation of enantiomer retention time in run-to-run, day-to-day and column-to-column experiments were 1.02, 4.45 and 5.60% using the (R)-(3,3′-di-p-cyanophenyl)-2,2′-dimethoxyl-1,1′-binaphthalene coated column, and 2.38, 3.20 and 4.94% using the (R)-(3,3′-dip-acetylphenyl)-2,2′-dimethoxy-1,1′-binaphthalene coated column. The results indicated that the (R)-1,1′-bi-2-naphthol derivatives may have utility in capillary electrochromatography.