Abstract: UHPLC-MS/MS was used for the determination of α,β,γ-hexabromocyclododecane (HBCD) in expanded polystyrene materials. The sample was extracted with acetonitrile,then separated on a Waters ACQUITY UPLC@BEH C18 column with the mixture of acetonitrile and 5 mmol·L-1 ammonium acetate solution as mobile phase for gradient elution. MRM was adopted for analysis in MS detection. The linear relationship was found between the peak area and the mass concentration of HBCD was in a certain range. The lower limit of detection (10S/N) was 0.2 mg·kg-1. The recovery rates measured by standard addition method were in the range of 81.7%-102%,with RSD (n= 7) less than 15%.