The Aburrá Valley region in Colombia, with Medellín as its main city, is an urban centre with about three million people. An investigation was carried out to deter-mine a set of baseline concentrations for VOC compounds associated with diesel fuel and gasoline, as vehicular emission tracers in the region. The VOC measurement campaigns, based on TENAX tube sampling and analysis according to TO-17 EPA method, were done in areas of low and high vehicular flow as well as on-board measurements covering major Medellín road networks during 24 hours. The results showed that there was a relation between VOCs concentrations and vehicular activi-ty. The diesel fuel sulfur content was also found as an important factor on VOC hy-drocarbon formation.