SummaryA critical study using C18 SPE columns for the determination of organophosphorus, triazine, and triazole-derived pesticides, napropamide, and amitraz is presented. The type of sorbent, sorbent mass, flow rate in the extraction process, sample concentration of the different compounds, sample volume, pH, and ionic strength were evaluated. Special emphasis was placed on the evaporation step of eluates prior to GC determinations and on prefiltration of sample waters. Pesticide recovery is linear over a wide range of concentrations for most of compounds under study. Under general extraction conditions losses can be expected for amitraz, prometryn, prometon, dimethoate, penconazole, and propiconazole. At 100 ng L-' , enhanced responses are produced for mevinphos, simazine, malathion, triadimefon, methidathion, and phosmet, which can be attributed to matrix effects. At basic pH, recovery of prometon, prometryn, and penconazole are improved. Low flow rates and high ionic strength enhance the recovery of prometon and prometryn. For phosmet, the influence of sample volume was established. Likewise, the influence of sorbent quantity was established for phosmet and dimethoate. Losses during the evaporation step were observed for mevinphos, dimethoate (1 50%), penconazole, propiconazole, and prometon (30%). Prefiltration of sample waters did not cause significant variations in the whole process of extraction. Impurities arising from the sorbent materials were not detected.