Ultrasonic/O3 combined process was employed to pretreat heterocyclic pesticide wastewater for increasing biodegradability and reducing biological toxicity. Influences of ultrasonic frequency, ultrasonic power, probe diameter, initial pH and O3 dosage on the COD removal were studied. The results showed that the ultrasonic/O3 process significantly improved the biodegradability and reduced the biological toxicity of the wastewater. The ratio of BOD5/COD was increased from 0.03 to 0.55 and the EC5o increased from 11% to 52% under ultrasonic/O3 treatment. Low ultrasonic frequency brought better COD removal. Initial pH was found to have a high influence on the COD removal and alkaline conditions were more favorable. The influences of ultrasonic power and probe diameter were small.With an increase in O3 dosage, COD removal was effectively improved. The optimal operational parameters for the combined process which the efficiency of COD removal reached 67.2%.