The aim of the present study was to attempt to describe a rapid procedure of purification and determination of the Zectran, Aminocarb and Bendiocarb in aqueous media using Reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to electrospray ionisation mass spectrometry (ESI). Different solids phases ODS sorbents were evaluated for the extraction of analytes in water. Sensitivity was evaluated by determining the limit of detection and recoveries of these compounds. The optimum conditions of extraction were applied for the screening of these substances in river water sample (Oued Madjerda). (C) 2009 Elsevier B.V. All rights reserved.