Abstract： Objective To establish a method to detect N-methylacetamide (NMAC) concentration in urine of workers occupationally exposed to NMAC with directly injecting the sample into capillary gas chromatography.Methods After frozen urine samples were isolated from precipitation by centrifugation,the aliquot of supernatant was pretreated by protein precipitation with dilution of methanol.The methanol supernatant was separated by Polyethylene Glycol (PEG)capillary columns and detected by nitrogen phosphoraus detector (NPD).Results Good linearity was obtained in the concentration range of 1.0～250 mg/L.The correlation coefficient was 1.0000.The minimum detection limit of NMAC in urine was 0.2 mg/L.The method recovery rates were 96.0％ ～ 99.4％ at three different concentrations.The mean recovery rate was 97.8％.The relative standard deviations (RSD) of intra- and inter-day were between 1.5％～3.4％.Conclusion The method was simple,rapid,selective and sensitive and was applicable to detect the urinary NMAC concentration for monitoring occupational exposure levels.