From April, 2008 to July, 2009, 187 atmospheric samples in four different seasons were collected from five sites in Shenyang. The 108 species of VOCs were measured by using the method of pre-concentration-GC-MS. The objectives of this study were to investigate the VOCs pollution level as well as its spatial and temporal distribution, and to identify the main source in Shenyang city. The results showed that the average total mass concentration of VOCs in Shenyang was 371.0 +/- 132.4 microg/m3. The major components were oxygen-containing compounds, halogenated hydrocarbon, alkanes, aromatics and alkenes, which accounted for 57.2%, 20%, 11.4%, 8.5%, and 3.0% of the total mass, respectively. A seasonal variation of VOCs across all the sampling sites was observed, with higher levels in spring and autumn and lower levels in winter and summer. Related with industrial emission, the diurnal variation of the total mean VOCs concentrations at downtown site showed three peaks in winter and two peaks in summer. The VOCs levels in the industrial and downtown areas were higher than those in other areas, with the lowest concentration observed at clean air site with no emission source around. From the results of correlation analysis and concentration ratios analysis, the VOCs pollutants in Shenyang were mainly contributed by automobile exhaust, coal & biofuel combustion, gasoline & solvent evaporation and industrial process.