In this research, a novel insoluble sorbent based on cyclodextrin and rigid aromatic groups tetrafluoroacetonitrile was designed for dispersive insoluble solid-phase extraction (DSPE). Due to its high adsorption capacity, this obtained polymer was applied to separation and concentration of trace quinolones in wastewater before HPLC determination. Various parameters influencing the extraction performance were studied and optimized. A DSPE approach coupled with high performance liquid chromatography was developed for the determination of four quinolones in wastewater samples. The limit of quantitation of fleroxacin, ciprofloxacin, gatifloxacin, norfloxacin were 2.67, 3.17, 4.75, 5.50ngmL−1, respectively. The recoveries of four quinolones range from 96.43 to 103.3% with relative standard deviations less than 4.5%. These results demonstrated that the proposed approach based on CDP was efficient, low-cost for extraction of quinolones from wastewater.