Solid phase micro extraction and gas chromatography mass spectrometry (SPME/GC-MS) was used to detect the ambient volatile organic compounds (VOCs) in Hefei Dongpu Reservoir, China, and the composition and variation characteristics of VOCs in the area were investigated. The result shows that these VOCs are mainly composed of benzene series, aldehydes, ketones and alkanes. Principal component analysis /absolute principal component scores (PCA/APCS) model was used to analyze the source of the VOCs. The result shows that there are 4 main sources of the VOCs, such as automobile emission sources account for 38.9%, chemical reagents sources account for 49.48%, industrial production sources account for 8.13% and medical alcohol evaporation sources account for 3.49%, respectiely.