Pollution of drinking water supplies from industrial waste is a result of several industrial processes and disposal practices, and the establishment of analytical methods for monitoring organic compounds related to environmental and health problems is very important. In this work, a method using solid-phase extraction (SPE) and gas chromatography coupled to triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) was developed and validated for the simultaneous determination of pesticide residues and related compounds in drinking and surface water as well as in industrial effluent. Optimization of the method was achieved by using a central composite design approach on parameters such as the sample pH and SPE eluent composition. A single SPE consisting of the loading on a polymeric sorbent of 100 mL of sample adjusted to pH 3 and elution with methanol/methylene chloride (10:90, v/v) permitted the obtaining of acceptable recoveries in most cases. The concentration factor associated with sensitivity of the chromatographic analysis permitted the achievement of the method limit of detection values between 0.01 and 0.25 μg L(-1). Recovery assays presented mean recoveries between 70 and 120% for most of the compounds with very good precision, despite the different chemical nature of the compounds analyzed. The selectivity of the method, evaluated through the relative intensity of quantification and qualification ions obtained by GC-QqQ-MS/MS, was considered adequate. The developed method was finally applied to the determination of target analytes in real samples. River water and treated industrial effluent samples presented residues of some compounds, but no detectable residues were found in the drinking water samples evaluated.