〔Abstract〕 Established Fe3O4@ZIF-67 magnetic dispersive micro-solid phase extraction(DMSPE) combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS) to determine 6 penicillins(PCs) in water samples residual method. Under the optimal extraction conditions, the detection limit of 6 PCs in water samples was 0.01～0.06 μg/L, and the limit of quantification was 0.03～0.19 μg/L; under the three concentration levels of 0.1, 1.0, 10.0 μg/L, the recovery rates of the 6 PCs in river water and aquaculture water samples were 79.2%～96.6% and 75.9%～94.8%, respectively; the matrix effect of the six PCs in river water and aquaculture water were 90.3%～102.2% and 89.6%～105.6%. Fe3O4@ZIF-67 has the ability to efficiently adsorb PCs. Combined with LC-MS/MS, it can realize the simultaneous rapid detection of 6 PCs in water samples.