Due to increasing concern about the assessment and protection of the quality of groundwater as a limited natural resource, an extensive monitoring program has been carried out, covering a highly agricultural area of Catalonia where different types of crops have been grown during the last 5-10 years. The paper reports the analytical protocol used (sampling, filtration, preconcentration, and analysis) and the most relevant organic compounds present in groundwaters from agricultural areas as well as the concentration levels found.