A hollow fiber supported liquid membrane extraction method for the liquid chromatographic determination of dinitrophenolic compounds at ppt levels has been developed. Different variables affecting the extraction process, such as extraction time, shaking speed, acceptor pH, acceptor buffer concentration, salt content and humic acids have been studied. Enrichment factors up to 7000 times were obtained. Validation of the method included calibration experiments and studies of the linearity of the responses in different matrices. Good linearity was obtained in the environmental matrices evaluated. Detection limits range from 6.0 to 8.0 ng/L, and the relative standard deviations do not exceed 7% in terms of repeatability.