Abstract: Toy sample (0.5 g) of textile fibrous material was extracted ultrasonically with acetone (10 mL) at 60 ℃ for 30 min. The extract was evaported to dryness by N2-blowing, and the residue was dissolved and made up to 5 mL with methanol. Toy sample (0.5 g) of plastic or rubber material was treated by soxhlet extraction with mixture of toluene and methanol (10+1) and the extract was evaporated to dryness. The residue was dissolved and made up to 5 mL with methanol. The methanol solution was used for UHPLC-MS/MS analysis. Chromatographic column of Acquity UPLC BEH C18 and mixture of (A) mixed solvent of CH3OH and CH3CN (4+1) and (B) 10 mmol·L-1 NH4OAc solution in the volumic ratio of 5 to 95 were used as stationary phase and mobile phase for separation of the 3 isomers of hexabromocyclododecane. Linearity ranges were found same between 1.0 to 2.0 mg·L-1 for the 3 isomers, with detection limits (3S/N) of 0.1, 0.2, 0.5 μg·L-1 respectively. Values of recovery found by standard addition method were in the range of 70.0%-112% with RSD′s (n=6) ranged from 0.070% to 9.9%.