AbstractA simple and rapid method for the determination of residues of four fluoroquinolones in blood samples was developed. The method was based on matrix solid‐phase dispersion extraction followed by CE with ultraviolet detection. 1‐Butyl‐3‐methylimidazolium tetrafluoroborate aqueous solution was used as the background electrolyte for the separation of fluoroquinolones. The average recoveries of the four fluoroquinolones at two spiked levels ranged from 54.0 to 86.4% for pig blood, and 45.4 to 79.9% for deer blood, with the relative standard deviations <9.45%. Detection limits for the four fluoroquinolones in blood sample ranged from 0.15 to 0.31 μg/mL.