Abstract: The sample (5.000 0 g) was extracted with ethyl acetate (20 mL+10 mL), and the combined extract was purified with 0.2 g of C₁₈ and PSA. After centrifugation, the organic layer was concentrated to 1 mL by N₂-blowing. The obtained solution was separated by GC using the polar capillary chromatographic column DB-624 UI and program temperature vent (PTV) large-volume sample-introduction at multimode inlet (MMI). Multiple reaction monitoring (MRM) mode was adopted in MS analysis. Linear relationships between values of peak area and mass concentration of N-nitrosamine compounds (N-nitrosodimethylamine, N-nitroso morpholine and N-nitrosodipropylamine) were found in the range of 1.0-40.0 μg·L^-1, with lower limits of determination (10S/N) of 0.75,0.39,0.28 μg·kg^-1, respectively. Tests for recovery were made by standard addition method for the representative meat product (ham sausage) and aquatic product (grilled fish), giving results in the range of 87.8%-103% and RSDs (n=10) all less than 8.0%.