Abstract: A graphene- based magnetic nanocomposite( Reduced graphene oxide / iron oxide,RGO / Fe₃O₄) was synthesized by one- pot solvothermal method and used as an effective adsorbent of magnetic solid- phase extraction,and then coupled with Gas Chromatography- Mass Spectrometer( GC- MS) for selective extraction and analysis of pyrethroid pesticides. Various experimental parameters affecting the extraction efficiencies were investigated.The optimized extraction conditions were studied.Finally,it was successfully applied to extraction and determination of pyrethroid pesticides in fruits and vegetables.Under the optimum conditions,the linear correlation coefficient ranged from 0.998 to 0.999. The results of RSD was 4.3% ~ 8.9% by testing five times.The limits of detection of the method were under 2.05 μg / kg. The recovery of the pesticides spiked in various real samples at three different concentrations ranged from 83.49% to 117.38%. These results indicated that as a magnetic solid-phase extraction adsorbent,RGO / Fe₃O₄ had a great potential for the preconcentration of pesticides from liquid samples.