Volatile organic compounds (VOCs) play a crucial role in modulating air pollution by ozone and fine particles, particularly in urban areas. While in recent years short-term intervention actions for better air quality during big events in China did present good opportunities to examine the effectiveness of control measures in reducing anthropogenic VOCs emission, it is highly challenging to interpret the real effect of a specific control measure based on field monitoring data when a cocktail of control measures were adopted. Here we took the air quality intervention actions during the 16th Asian Games (AG) in Guangzhou as a case study to explore the impact of short-term multiple measures on VOCs reduction. The average mass concentrations of VOCs decreased by 52-68% during the AG. These percentages could not reflect emission reduction rates as the concentration might be also heavily impacted by dispersion conditions. Diagnostic ratios, such as methyl tert-butyl ether to carbon monoxide (MTBE/CO) and i-pentane/CO, decreased by over 60% during the AG, suggesting a substantial reduction in gasoline related emissions. A method linking emission reduction rates of two sources with their contribution percentages before and during the AG by using a receptor model was further formulated. With the available reduction rate of 34% for vehicular exhaust obtained during the traffic restriction drill in our previous study, VOCs emissions from gasoline evaporation and solvent use reduced by 45.7% and 13.6% during the AG, respectively. Total VOCs emissions decreased by 25.3% on average during the AG, and the emission control of vehicular exhaust, oil evaporation, and solvent use accounted for 17.0%, 6.3% and 2.0% of total VOCs emission reduction, respectively. This study presented an observed-based method with diagnostic/quantitative approaches to single out the effectiveness of each control measures in reducing VOCs emissions.