Abstract: The composition and concentrations of volatile organic compounds (VOCs) in ambient air in Hockey Field District, Macao have been studied and reported in this paper. The main VOCs are BTEX, and the average concentration of total BTEX is 57.2 μg/m³,which is higher than those in most other cities in the world. The study of VOCs in urban air in Hockey Field District indicates that the concentrations of VOCs in urban air depend on topography and climate conditions of the sampling point.