A simple, rapid and eco-friendly method named dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) was developed for the determination of 2-tert-butyl-4-ethylphenol, 4-tert-octylphenol and 2,4-di-tert-butylphenol in wastewater samples coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV).Octanoic acid was served as extraction solvent, and methanol was selected as dispersive solvent.The parameters affecting the extraction efficiency including the type and volume of the extraction solvents and the dispersive solvents, the pH and the salt addition were optimized.Under optimum conditions, the linear range was 20-1500 μg/L for all the three target alkylphenols.Limits of detection (LODs, S/N=3) were in the range of 0.45-0.61 μg/L.The enrichment factors (EFs) varied from 145 to 169, and the recoveries at three spiked levels were in the range of 80.1%-109.9%.It demonstrated that fatty acids including octanoic acid and nonanoic acid could be used as extraction solvent in DLLME-SFO method.The method is suitable for the determination of alkylphenols in environmental water samples.