Abstract: Gas chromatography-secondary mass spectrometry was applied to the determination of residual acrylamide in 4 kinds of foodstuffs,i.e.potato strips or chips,coffee,biscuits and pop-food.Acrylamide in sample was extracted with water at room temperature,and the aqueous phase was centrifuged and defatted with n-hexane,and then purified by the Supleco Envi-Cabr SPE column.A precolumn derivatization of acrylamide was performed by bromination with KBr,HBr and saturated bromine water to form the volatile compound of 2,3-dibromopropionamide,which was separated and determined by the GC-MS/MS.Linearity between the peak area and concentration of acrylamide was obtained in the range of 10-1 000 μg·L-1 (r=0.999),with its detection limit (3σ) of 4.02 μg·kg-1.External standard method was used in the quantitative analysis.Precision and recovery were tested by adding the standard acrylamide of 3 different concentration levels (10,100,1 000 μg·kg-1) to 3 kinds of foodstuff samples,and analyzed by the proposed method,values of RSD′s (n=8) and recovery found were in the range of 8%-12% and 68.3%-105.2% respectively.The proposed method was suitable to be used in analysis of samples in batches,for its features of selectivity sensitivity and rapidity.