A novel magnetic solid phase extraction (SPE) analysis method was established by combining Fe3O4 magnetic nanoparticles modified grapheme as absorption material followed by GC/MS for detection of the organochiorine pesticide (OPs) in water. Magnetic nanoparticles modified grapheme (MNG) was prepared by graphene oxide (GO) and Fe2+ through redox reaction in one step. Then, cationic surfactant CTAB was added as micelle forming agent, in which MNG was carrier of mixed micelles extraction system. Mixed micelle modified MNG has higher loading capacity than pure Fe3O4 magnetic graphene. This method was applied to analysis of Ops in water source. The detection limit was in the range of 1.5-5.0 ng/L. The recovery was ranged from 67.2% to 95.6%. The RSD of repeatability was lower than 9.9%. As compared with ordinary SPE, the sensitivity of new method increased 50-109 times.