The chemical speciation of Volatile Organic Compounds (VOCs) in the air of the Huayuan region, Tianjin is analyzed by using the GC-MS with pre-concentration of three-level cold trap. A total of 108 VOCs species are detected. The major components are alkanes and aromatics which account for 59.2% of VOCs. The average mass concentration range of VOCs in the winter and spring is 519.4—1029.6μg/m³, 299.8—463.8μg/m³, respectively. Among them, the acetone has the maximum concentration (20.0μg/m³); meanwhile the heptane has the minimum concentration (1.1μg/m³). The average mass concentration of VOCs and individual substances are higher in the winter than that in the spring. It could be explained by the seasonal variation of atmospheric degradation and dilution, while another important reason is that the surrounding pollutant sources due to atmospheric transport have an effect on Huayuan region.