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Dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography "mass spectrometry" (GC/MS) was applied for the determination of 11 alkylphenols in eluates of chars produced in the co-pyrolysis of different wastes. The optimized DLLME procedure, 4mL of sample solution, 15 mu L of trichloroethylene as extraction solvent, 1mL of acetone as dispersion solvent and addition of 15% (w/v) of NaCl, was validated. Under the optimum conditions, the enrichment factors were in the range of 82-180. Calibration curves were constructed for each analyte in pure water in the concentration range of 0.5-0.8 mu g/L with correlation coefficients higher than 0.999. The limits of detection were between 0.07 and 0.17 mu g/L. The repeatability of the method was evaluated using water samples fortified with the analyte mixture at two concentration levels: the relative standard deviation (RSD) values were between 3.7% and 8.0% for a concentration of 0.5 mu g/L, and between 4.2% and 6.4% for a concentration of 3 mu g/L. The recoveries of the analytes evaluated by fortification of real eluate samples were in the range of 67.9-97.9% for eluate 1 (obtained from a decontaminated char) and in the range of 61.9-101.4% for eluate 2 (obtained from the untreated char). Methylphenol presented low recoveries for both eluates showing a possible matrix effect. The results obtained show that this method is adequate for the determination of alkylphenols in environmental aqueous samples and presents itself as a fast and inexpensive technique, using minor amounts of organic solvents.