The Monterrey Metropolitan Area (MMA) has shown high concentration of PM2.5 in its atmosphere since 2003. The contribution of possible sources of primary PM2.5 and its precursors is not known. In this paper we present the results of analyzing the chemical composition of sixty 24-hour samples of PM2.5 to determine possible sources of PM2.5 in the MMA. The samples were collected at the northeast and southeast of the MMA between November 22 and December 12, 2007, using low-volume devices. Teflon and quartz filters were used to collect the samples. The concentration of sixteen airborne trace elements was determined using X-ray fluorescence (XRF). Anions and cations were determined using ion chromatography. Organic carbon (OC) and elemental carbon (EC) were determined by thermal optical analysis. The results show that Ca had the maximum mean concentration of all elements studied followed by S. Enrichment factors above 50 were calculated for S, Cl, Cu, Zn, Br, and Pb. This indicates that these elements may come from anthropogenic sources. Overall the major average components of PM2.5 were OC (41.7%), SO4-2 (22.9%), EC (7.4%), crustal material (11.4%), and NO3- (12.6%), which altogether accounted for 96% of the mass. Statistically, we did not find any difference in SO4-2 concentrations between the two sites. The fraction of secondary organic carbon was between 24% and 34%. The results of the factor analysis performed over ten metals and OC and EC show that there are three main sources of PM2.5: crustal material and vehicle exhaust; industrial activity, and fuel oil burning. The results show that SO4-2, OC, and crustal material are important components of PM2.5 in MMA. Further work is necessary to evaluate the proportion of secondary inorganic and organic aerosol in order to have a better understanding of the sources and precursors of aerosols in the MMA.