The application of TLC with a diode array detector (TLC-DAD) and HPLC-DAD after SPE for identification and quantitative analysis of pesticides in water samples is demonstrated. The procedures described for the determination of compounds are inexpensive and can be applied to routine analysis of analytes in water samples after preliminary cleanup and concentration by SPE. Average recoveries for four different cartridges and three solvents by the proposed HPLC-DAD method after SPE also are presented. The efficiency of the SPE procedure was evaluated using real water samples from the Zemborzycki Reservoir, near Lublin, southeastern Poland. The method was validated for precision, repeatability, and accuracy.