Abstract: A method for the simultaneous determination of nine N-nitrosamine in pickling dried fish was developed by gas chromatography-hydrogen flame detector(GC-FID)with by lye heating treatment combined with dichloromethane extraction. The filtrate was purified by coconut shell activated carbon,and concentrated by C₁₈ SPE columns;the chromatographic separation were carried with a DB-WAXETR polar column(30 m×0.25 mm,0.25 μm). The column temperature was programmed to rise. Results showed that:The Nine nitrosamines had good linearity in the range of 0.05~5 μg/mL(R²>0. 999);The detection limits and quantitation limits were ranged from 0.05 to 0.29 μg/mL and 0.18 to 0.95 μg/mL. The recoveries and RSD were 76.8%~129.5% and 2.29%~15.5%. The actual sample detection result in 50 kinds of pickled dried fish showed that the detection rates of NDEA,NDIP and NPYR were 20%,20% and 24%. Only one sample exceeded the national standard limit(NDMA<4 μg/kg).