Neste trabalho propõe-se método rápido de procedimentos de extração e clean up para determinações do inseticida Metamidofós em amostras de soja. Análises de amostras de soja seca e hidratada, fortificadas em níveis de 5 µg g-1, apresentaram recuperação média de 93-94% e coeficiente de variação de 17 a 31% com os sistemas adsorvente alumina/florisil e eluente metanol/ acetonitrila 1:3. Testes empregando sílica 15% desativada também mostraram eficiência com recuperação final de, aproximadamente, 75% e coeficientes de variação entre 18 a 27%. Cromatogramas com mínima interferência, nenhum efeito de matriz e boa eficiência na extração foram obtidos com a aplicação do método proposto. METHAMIDOPHOS INSECTICIDE RESIDUE ANALYSIS IN SOYBEAN AND FINAL DETERMINATION BY GAS CHROMATOGRAPHY Abstract A rapid method for extraction and clean up procedures for methamidophos insecticide determinations in soybean samples is proposed in this work. Analyses of dried and natural soybean samples fortified at 5 µg g-1 level showed recoveries average of 93-94% and variation coefficient ranging from 17 to 31% by using 3:1 Alumina/Florisil adsorbent system combined with 1:3 methanol/acetonitrile as eluent system. Tests employing 15% deactivated silica also showed to be efficient with final recovery close to 75% and variation coefficients varying from 18 to 27%. Chromatograms with minimal interferences, no matrix effects and good extraction efficiencies were recorded after application of the proposed method.