Abstract: The water samples were collected with brown sampling bottles, and 80 mg of sodium thiosulfate and 5 mL of methanol were added to each liter of the water sample. 1 L of the treated sample was taken, and 20.0 μL of 1.00 mg·L⁻¹ extraction internal standard （carbon isotope labeled target compounds were used as extraction internal standards） solution was added. After mixing well, the sample was suction-passed through a 0.45 μm filter membrane, and the filtrate was collected. The suction-filtered filter membrane was cut into pieces and placed in a 15 mL-centrifuge tube. 5 mL of acetone was added, and the mixture was extracted by ultrasound for 20 min and passed through a 0.45 μm polytetrafluoroethylene (PTFE) needle filter. The filtrate was combined with the previously suction-filtered filtrate and the mixture was passed through a ChromP solid phase extraction column (activated successively with 10 mL of dichloromethane, 10 mL of acetone, 10 mL of methanol and 10 mL of water). The solid phase extraction column was purged with nitrogen for 10 min and eluted with 15.0 mL of the mixed solution of dichloromethane and acetone at a volume ratio of 9∶1. The eluate was collected and blown to near dryness with nitrogen, and the residue was dissolved and made its volume up to 1.0 mL with methanol. 20.0 μL of 1.00 mg·L⁻¹ injection internal standard deuterated isotope labeled α-hexabromocyclododecane (α-HBCD) was used as injection internal standard solution was added, and after mixing well, the solution was passed through a 0.22 μm PTFE needle filter. The 3 hexabromocyclododecanes (HBCDs) including α-HBCD, β-HBCD and γ-HBCD,and tetrabromobisphenol A (TBBPA) in the filtrate were determined by liquid chromatography-tandem triple quadrupole mass spectrometry. Extend C₁₈ column was used as the stationary phase and the mixed solution composed of water and organic phase (a mixed solution of methanol and acetonitrile at a volume ratio of 1∶1) at different volume ratios was used as the mobile phase for gradient elution. Electrospray ion (ESI) source was used for mass spectrometry. The targets were analyzed by multiple reaction monitoring (MRM) mode in negative ion (ESI⁻) scanning mode. As shown by the results, the mass concentration ratios of 4 target compounds in the range of 2.00-200 μg·L⁻¹ to the extraction internal standards were linearly related to the ratios of their corresponding response intensities, with detection limits (3.143s) in the range of 0.5-0.8 ng·L⁻¹. Test for recovery was made by the standard addition method, giving results in the range of 88.4%-129%, with RSDs (n=6) of the determined values in the range of 2.3%-15%. This method was used for the analysis of 32 surface water samples and 2 wastewater samples, and the target compounds were not detected in 29 surface water samples. The detection amounts of HBCDs were in the range of 0.5-1.9 ng·L⁻¹, and the detection amounts of TBBPA were in the range of 1.4-17.8 ng·L⁻¹ in the remaining samples.