In this study, boehmite nanoparticles were used for the extraction of chlorophenols, 2,4- dichlorophenol, 2,6- dichlorophenol and 2,4,6- trichlorophenol from real aqeous samples by head space- solid phase microextraction using derivatization. This adsorbent interaction strongly with target species due to the presence of numerous hydroxyl functional groups at its surface which results in the extraction of compound. Gas chromatography equipped with electron capture detector (ECD) was used to isolate and identify analytes. Different parameters affecting the extraction efficiency including, derivatization reagents, ionic strength, desorption temperature, desorption time, equilibrium time, desorption temperature and equilibrium temperature were examined. The limit of detection studied under optimum conditions was 9.0, 13.0, 0.3 ng/L for 2,4-dichlorophenol, 2,6-dichlorophenol and 2,4,6-trichlorophenol, respectively. The linear ranges were obtained for 2,4-dichlorophenol, 2,6-dichlorophenol and 2,4,6-trichlorophenol 0.05-5, 0.05-5 and 0.003-0.1 ?g/L, respectively. The relative standard deviation obtained in this study was obtained in the range of 2.2-11.8. Compared to other methods for measuring chlorophenols in aqueous samples, improved efficiency, lower analysis cost and lower organic solvent consumption were obtained. The fiber was prepared, has better efficiency than commercial fiber (CAR-PDMS). In this study, chlorophenols were measured in aqueous real samples including aqueous samples of Anzali wetland, inlet effluent and outlet effluent of a plant a factory with recovery percentage in the range of 99-110.