Abstract: A high performance liquid chromatography-triple quadrupole mass spectrometry method was developed to determine three hexabromocyclododecane (HBCD) isomers and tetrabromobisphenol A (TBBPA) in soil and sediment, for the needs of the Stockholm Convention on Persistent Organic Pollutants and new pollutants control in China. Samples were freeze-dried, extracted by pressurized fluid with n-hexane and acetone (volume ratio, 1∶1), and then cleaned up with neutral and acidic silica gel columns. They were quantitated by instrumental analysis using isotope dilution method. The results showed that: (1) Effective baseline separation was achieved by liquid chromatography, and the retention time was stable with relative deviation less than 3.0%. The relative standard deviation of the average relative response factor was less than 15% in the concentration range of 2.0-200 ng/mL. (2) The detection limits for α-HBCD, β-HBCD, γ-HBCD and TBBPA were 0.06, 0.04, 0.04 and 0.06 μg/kg, respectively. (3) The precision of the method was 1.76%-10.6%, and the recovery was 92.9%-121%. (4) Spiking experiments were carried out on eight soil types with different pH value. The recovery ranged from 85.9% to 104%. The established method has demonstrated high sensitivity and high applicability, and can be used for the determination of HBCDs and TBBPA in complex soil and sediment samples.