Abstract: The residues of Ethinylestradiol，Diethylstilbestrol，4-Nonylphenol and Estradiol benzoate in food were determined simultaneously by SPE-HPLC．The samples were ultrasonic extracted with acetonitrile，centrifuged，concentrated and purified by C18 solid phase extraction column，analyzed with the HPLC method． This study optimized the conditions of SPE，and four components were well separated. The detection limit of the method was ranged from 6 to 12 μg/kg． The recovery rates were 80. 3%～107. 8%. The calibration curves were linear with correlation coefficient ranged from 0.998 8 to 0.999 8． The relative standard deviations were 0. 124%~1. 72%. This method has high sensitivity，fine separability，simple sample preparation，and can reduce the inteference of impurities，which is satisfied with the estrogen analysis.

Key words: solid phase extraction, HPLC, trace estrogen, food detection