An ultrasonic extraction-solid phase extraction-reversed phase high performance liquid chromatographic method was developed to determine sulfonamides and tetracyclines antibiotics in surface sediments by optimizing condition of pretreatment.The sediment samples were extracted with a mixture of methanol-EDTA/McIlvaine buffer(1∶1) under ultrasonication after freeze-dried,then blowed at 40 ℃ under nitrogen to remove the organic solvent.After purified with a Poly-Sery HLB solid-phase extraction cartridge,the extract was determined with ODS-P C18 column and UV-detector.The results showed that the calibration curves of 7 sulfonamides were linear(r2>0.999) in the concentration range of 0.025-0.5 mg/L,and the recoveries of three spiked levels ranged from 71.4% to 107.6% with relative standard deviations(RSDs,n=3) of 14%-52%.The method detection limits(MDL) ranged from 0.07 ng/g to 0.29 ng/g.The calibration curves of 3 tetracyclines were linear(r2>0.999) in the concentration range of 0.05-1 mg/L,the recoveries at three spiked levels ranged from 62.2% to 87.9%,with RSDs(n=3) of 1.1%-4.6%,and the method detection limits(MDL) were in the range of 0.45-0.58 ng/g.The developed method was applied to analyze the surface sediments of an urban lake and its inflowing rivers,in which 10 kinds of target antibiotics were all detected.The results showed that the method was simple,rapid and accurate,and was suitable to determine the sulfonamides and tetracyclines antibiotics in the sediments.