Abstract: A method of capillary electrochromatography was proposed for the resolution of enantiomers of deltamethrin using allyl-β-cyclodextrin chiral monolithic capillary column as separation column, which was prepared by in-situ polymerization. A mixed solution of acetonitrile and 5 mmol·L-1 NaH2PO4 (of pH 6.5) solution (40+60 by vol.) was used as mobile phase. Separation voltage of 10 kV and capillary column temperature of 20℃ were chosen. Under the optimized conditions, 4 pairs of enantiomers of deltamethrin were successfully separated within 10 min.