A survey of the herbicides present in surface and groundwaters was conducted in 1999 in an area of the provinces of Salamanca and Zamora (Central-Western Spain) to assess the degree of pollution of the agricultural land and seasonal changes in the presence of herbicide residues. Ten sites were sampled and screened for 17 herbicides commonly used in the area; the compounds were ureas, triazines, amides, and others. A previously optimised method involving solid-phase extraction with polymeric cartridges, followed by HPLC with diode array detection, was used to monitor the herbicides. Of the 17 compounds examined, eight were found: chlorotoluron (41% of total detections), terbutryn (21%), atrazine (14%), linuron (7%), isoproturon and metolachlor (5.5% each), lenacil (4%) and metamitron (2%). Of the detections, 66% corresponded to river water samples (three sites). The herbicides found in groundwaters (seven sites) were: chlorotoluron, atrazine, terbutryn, linuron, and isoproturon, all of which are classified as probable or transient leachers in Europe. The temporal evolution of the herbicide content in river waters shows that the observed pollution is a function of time and is related to the application and use of the herbicides. By contrast, the pollution found in groundwaters was lower than that seen in surface waters, except that due to chlorotoluron, which, additionally, remained almost constant throughout the study period.