The majority of the methods developed to date for the determination of PUHs in vegetables, fruits and soils are based on the direct extraction with methanol, being the co-extractives removed by partitioning (with other solvents) and then cleaned-up on sorbents with acetone or acetonitrile as eluents. Therefore, these methods are characterized by the high consumption of organic solvents; only one method has been proposed for the determination of linuron in aqueous soil extracts by LC [23]. In this work, phenylurea herbicides are extracted from plant materials using an aqueous medium, thus avoiding the hazard and high cost of organic solvents; additional steps, such as preconcentration and clean-up, are performed in a continuous manner using a SPE system. The sole organic solvent used was ethyl acetate both as eluent and in the washing of the sorbent column. The sensitivity and selectivity of the GC/MS technique allows the screening of these herbicides at ng g−1 levels in plants.