Abstract: A high performance liquid chromatography-triple quadrupole mass spectrometry method was developed to determinate three hexabromocyclododecane (HBCD) isomers and tetrabromobisphenol A (TBBPA) in soil and sediment, for the needs of Stockholm Convention and emerging pollutants monitoring in China. The samples were freeze-dried, extracted by pressurized fluid with n-hexane/acetone (V/V, 1/1), and then cleaned up by neutral and acidic silica gel column. After analyzed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS), they were quantitated by isotope dilution method. The results showed that: ① effective baseline separation was achieved by liquid chromatography, and the retention time deviation was less than 0.13 min. The relative standard deviation of the mean relative response factor was less than 15% in the concentration range of 2-200 ng/mL. ②The limits of detection of α-HBCD, β-HBCD, γ-HBCD and TBBPA were 0.06, 0.04, 0.04 and 0.06 μg/kg, respectively. ③The precision of the method was 0.56%~10.6%, and the recoveries was 92.9%~121%. (4) The addition experiment was carried out with 8 different soil types and regions. The recoveries ranged from 85.9% to 104%. (5) The established method has demonstrated high sensitivity and strong robustness, and could be applied to the determination of HBCDs and TBBPA in complex soil and sediment samples.