Abstract: A method for the simultaneous determination of migration of trace As and Sb in food contact materials by sequential injection-hydride generation-atomic fluorescence spectrometry with L-cysteine as a prereductant was developed.The influence factors such as L-cysteine, the acidity of sample solution and carrier liquid, the concentrations of NaBH4 and the interference of coexistent elements were investigated. The detection limits were 0.038 and 0.040μg/L, the LOQ were both 0.0010mg/L, the recoveries were in the ranges of 95.6%～102% and 96.3%～103%, and the relative standard deviations were 2.64%～4.09% and 2.33%～4.18% (n=8) for As and Sb respectively. The method was sensitive, simple, quick and accurate, which could be used for determination of migration of trace As and Sb in food contact materials.