Objective To establish a GC-MS method of simultaneous determination of fluoroacetamide and tetramine in food. Methods Target compound was extracted by acetronitrile, then separated by DB-WAX capillary column and detected by single quadrupole mass spectrometry. Retention time and characteristic ions were used as qualitative evidence, and external standard was used for quantification. Results The linear range for fluoroacetamide and tetramine was 0.05~10.0 mg/L and 0.01~10.0 mg/L (r>0.999), the limit of detection was 0.04 mg/kg and 0.01 mg/kg, and the average recoveries was 60.0~79.4% and 68.2~92.5%. Conclusion The method is sensitive, convenient, accurate and reliable. It is suitable for rapid determination of fluoroacetamide and tetramine in food.