Abstract:A quick, easy, cheap, effective, rugged and safe(QuEChERS) method coupled with ultra performance liquid chromatographytandem mass spectrometry (UPLCMS/MS) was established for the determination of hexabromocyclododecane (HBCD) in fish. QuEChERS method was used for sample pretreatment. The chromatographic separation was performed on a C18 column by gradient elution with water (mobile phase A) and methanolacetonitrile solution (mobile phase B, volume ratio =50∶50) as mobile phase. UPLCMS/MS method was used for MS/MS analysis with electrospray ion source in negative mode under multiple reaction monitoring mode, and isotope dilution internal standard method was used for quantification. The method had a good linear relationship in the concentration range of 0.5~50 μg/L (r≥0.999). The limits of detection (LOD) were in the range of 005~0.27μg/kg. The recovery rates of the three concentrations (2.5, 12.5, 25 μg/kg) were in the range of 99.3%~107%. The relative standard deviations were 0.4%~8.4%. The method is simple, accurate and sensitive, and can meet the detection requirements of HBCD in fish.