The Monterrey Metropolitan Area (MMA) in Northeast Mexico has shown high PM2.5 concentrations since 2003. The data shows that the annual average concentration exceeds from 2 to 3 times the Mexican PM2.5 annual air quality standard of 12 μg/m3. In a previous work we studied the chemical characterization of PM2.5 in two sites of the MMA during the winter season. Among the most important components we found ammonium sulfate and nitrate, elemental and organic carbon, and crustal matter. In this work we present the results of a second chemical characterization study performed during the summer time and the application of the chemical mass balance (CMB) model to determine the source apportionment of air pollutants in the region. The chemical analysis results show that the chemical composition of PM2.5 is similar in both sites and periods of the year. The results of the chemical analysis and the CMB model show that industrial, traffic, and combustion activities in the area are the major sources of primary PM2.5 and precursor gases of secondary inorganic and organic aerosol (SO2, NOx, NH3, and volatile organic compounds [VOCs]). We also found that black carbon and organic carbon are important components of PM2.5 in the MMA. These results are consistent with the MMA emission inventory that reports as major sources of particles and SO2 a refinery and fuel combustion, as well as nitrogen oxides and ammonium from transportation and industrial activities in the MMA and ammonium form agricultural activities in the state. The results of this work are important to identify and support effective actions to reduce direct emissions of PM2.5 and its precursor gases to improve air quality in the MMA. Implications: The Monterrey Metropolitan Area (MMA) has been classified as the most airpolluted area in Mexico by the World Health Organization (WHO). Effective actions need to be taken to control primary sources of PM2.5 and its precursors, reducing health risks on the population exposed and their associated costs. The results of this study identify the main sources and their estimated contribution to PM2.5 mass concentration, providing valuable information to the local environmental authorities to take decisions on PM2.5 control strategies in the MMA.