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In this study, monodisperse magnetic carbon microspheres were successfully synthesized through the carbonization of phenolic resin encapsulated Fe3 O4 core-shell structures. The magnetic carbon microspheres showed high performance in ultrafast extraction and separation of trace triazine herbicides from environmental water samples. Under optimized conditions, both the adsorption and desorption processes could be achieved in 2 min, and the maximum adsorption capacity for simazine and prometryn were 387.6 and 448.5 μg/g. Coupled with HPLC-UV detection technology, the detection limit of triazine herbicides was in the range of 0.30-0.41 ng/mL. The mean recoveries ranged from 81.44 to 91.03% with relative standard deviations lower than 7.47%. The excellent magnetic solid phase extraction performance indicates that magnetic carbon microspheres are promising candidate adsorbent for the fast analysis of environmental contaminants. This article is protected by copyright. All rights reserved.