Objective An analytical method for determination of five N-nitrosoamine in water samples was developed using solid-phase extraction and gas chromatography/mass spectrometry (SPE-GC-MS/MS). Methods The samples were pretreated with Cleanert pesticarb SPE solid phase extraction column, then separated by DB-35MS(30 m×0.25 mm,0.25 μm) chromatographic column under, select ion scanning mode(SIM). The determination of five N-nitrosoamine in drinking water by gas chromatography-mass spectrometry method was established by the optimization of ion effect, pH and eluent flow rate. Results The result showed that all five N-nitrosoamine had good linearities in the range of 0.05 to 1.00 μg/ml,the detection limits for 5 nitrosamines were 0.001,0.001,0.000 5,0.02 and 0.002 μg/L(S/N=3). The average recovery rates measured by standard addition method were in the range of 70.32%-96.39% with the relative standard deviation (n=6) in the range of 2.98%-5.29%. Conclusion The method had high sensitivity, wide linear range and optimized the detection conditions of five N-nitrosoamine in drinking water, and it was suitable for the detection of N-nitrosodamine in drinking water.