Abstract: A method was developed for the simultaneous analysis of PCBs and OCPs in sludges from the Yangtze River Delta Region of China by gas chromatography with electron capture detection (GC-ECD). The method involved was activated by ultrasonic extraction using acetone and petroleum ether, clean-up with sulfuric acid, copper power treatment and silica gel column chromatography. The test results with this method showed that the recovery (57.21%~101.51%), relative standard deviation (1.89%~14.67%) and detection limits (0.09~0.33 滋g/kg) could be satisfactorily obtained. This method was also cost-effective and did not require large amount of sludge sample. It could determine PCBs and OCPs in the same extract with enough accuracy, sensitivity and permissible RSD. PCBs and OCPs in the municipal sludges derived from the Yangtze River Delta Region of China were detected with this method.