The goal of this work was the development of a methodology based on solid phase extraction (SPE) to characterize nitrogen compounds and phthalates from landfill leachate samples. Activated carbon (AC) was used to extract all the organic compounds from the samples. The samples were collected in Porto Alegre-South Brazil. As the AC used had small particle size, it was impossible to use it in the form of packed cartridges; hence, it had to be applied in a batch mode. The desorption of the organic compounds from the AC was made by sonication with dichloromethane. The extract was analyzed by gas chromatography with mass spectrometric detection (GC-MSD). Some aspects of the validation of the methodology were also established. Several nitrogen compounds and phthalates were identified in the samples, proving the efficiency of this method with regard to the selectiveness for these substances.