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This study aimed to develop a new extraction method to analyze persistent organic pollutants (POPs) in the sediment of the Billings Dam in São Paulo, via gas chromatography with mass spectrometry (GC/MS). The Stockholm Treaty, held in Sweden in 1972, sponsored by the UN, with 113 participating countries, including Brazil, aimed to eliminate at least twelve POPs, thus contributing to the environmental issue. POPs are compounds that persist in the environment and are highly stable, being able to cross the placental barrier. Aldrin, Endrin, Dieldrin, DDT. DDE, DDD and Heptachlor. In order to guarantee the reliability of the analytical results, method validation tests were carried out, based on INMETRO guidelines. The Quechers method was used to extract the analytes, obtaining recovery results of between 40 and 120% for all the POPs analyzed in this work, acceptable values for complex matrices such as sediment. The limits of detection and quantification were 0.3 and 0.5 µg/kg respectively. The samples analyzed showed no significant contamination by POPs according to current Brazilian legislation.