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The occurrence of 26 commonly used cytostatic compounds in wastewaters was evaluated using an automated solid-phase extraction (SPE) method with liquid chromatography-high-resolution mass spectrometry (LC-HRMS). Detection was optimized using Oasis HLB SPE cartridges at pH 2. Two hospital effluents and their two receiving wastewater treatment plants were sampled over five days. In hospital effluents, eight cytostatics were detected at levels up to 86.2 mu g L-1 for ifosfamide, 4.72 mu g L-1 for cyclophosphamide, and 0.73 mu g L-1 for irinotecan, the three most relevant compounds identified. Cyclophosphamide and megestrol acetate were found in wastewaters at concentrations up to 0.22 mu g L-1 for the latter. The predicted environmental concentrations (PEC) in sewage effluents of ifosfamide (2.4-4.3 ng L-1), capecitabine (11.5-14.2 ng L-1), and irinotecan (0.4-0.6 ng L-1), calculated from consumption data in each hospital, published excretion values for the target compounds, and wastewater elimination rates, were in agreement with experimental values.