In this work,a reliable and sensitive method for detecting polybrominated diphenyl ethers(PBDEs) has been developed by the combination of liquid–liquid extraction and gas chromatography–mass spectrometry.PBDEs were extracted from a large volume of water by liquid–liquid extraction and purified by silica gel chromatography.In order to reduce the deviation,dibromobiphenyl was exploited as the internal standard to minimize differences among the injections.The quantification was performed using an external standard.Good linear correlation coefficients(>0.991) and a wide linearity range(1.0–500.0 ng/L) indicated the steadiness of the proposed method.Moreover,the satisfactory recovery(>75%)suggested that successful determination of PBDEs in river water had been achieved.Furthermore,the deduction behavior of PBDEs in river water could be inferred according to the results. In this work, a reliable and sensitive method for detecting polybrominated diphenyl ethers (PBDEs) has been developed by the combination of liquid-liquid extraction and gas chromatography-mass spectrometry. PBDEs were extracted from a large volume of water by liquid-liquid extraction and purified by silica gel chromatography. Order to reduce the deviation, dibromobiphenyl was exploited as the internal standard to minimize differences among the injections. quantification was performed using an external standard. Good linear correlation coefficients (> 0.991) and a wide linearity range ( 1.0-500.0 ng / L) indicates the steadiness of the proposed method. Moreover, the satisfactory recovery (> 75%) suggested that successful determination of PBDEs in river water had been achieved. Future and the deduction behavior of PBDEs in river water could be inferred according to the results.