To illustrate the major sources responsible for the redox activity of ambient fine particles during the 2014 Asia-Pacific Economic Cooperation (APEC) conference in Beijing, 3 months of daytime (8:00-19:30 LST) and nighttime (20:00-7:30 LST) particulate kmatter (PM2.5) was collected in Huairou, Beijing from November 3, 2014 through January 31, 2015. PM2.5 compositions were analyzed, including elements, organic carbon, elemental carbon, water-soluble ions, organics, and redox activities measured by both the dithiothreitol and the macrophage reactive oxygen species (ROS) assays. The mass-normalized redox activity was approximately constant during the noncontrol period (NCP) and control period (CP). The absolute value of the volume-normalized redox activity was about 4 times higher during NCP than that during CP, indicating the effectiveness of the control measures. The statistical analysis results showed that an interquartile range increase in PM2.5 mass, chemicals, and sources (μg/m3) was associated with the 1-3% increase in redox activity, indicating that the successful control did make a significant reduction in redox activity but did not elucidate that some source controls (i.e., vehicle emissions) could be more effective at reducing redox activity than other control programs (i.e., dust source). This study demonstrated that combustion particles from both solid fuels and liquid fuels could contribute to ROS generation. Furthermore, ROS could be formed in the atmosphere via photochemical reactions, which highlights the need to further research on their formation pathways. A better understanding of the relevant mechanistic pathways and different source contributors to ROS will help to guide strategies for targeted mitigation of the atmospheric oxidation potential and will also help to reduce the great disease stress caused by exposure to air pollution.