Residues of tetra-cycline antibiotics(TCs) in envi-ronments may be harmful to human.Due to their high polarities,it is ex-tremely challenging to efficiently enrich TCs with low concentrations in natural waters for analysis.In this work,a magnetic metal-organic framework Fe3O4@[Cu3(btc)2]was synthesized and applied as a dispersive micro-solid phase extraction adsorbent for TCs enrichment.Effects of dispersive micro-solid phase extraction conditions including extraction time,solution pH,and elution solvent on the extraction efficiencies of TCs were investigated.Results show that TCs could be enriched efficiently by Fe3O4@[Cu3(btc)2],and electrostatic interaction between TCs and Fe3O4@[Cu3(btc)2]dominated this process.Combined with liquid chromatography-tandem mass spectrometry,four TCs residues (oxytetracycline,tetracycline,chlortetracycline,and doxycycline) in natural waters were determined.The detection limits (LOD,S/N=3) of the four antibiotics were 0.01-0.02 μg/L,and the limits of quantitation (LOQ,S/N =10)were 0.04-0.07 μg/L.The recoveries obtained from river water and aquaculture water spiked with three TCs concentration levels ranged from 70.3％ to 96.5％ with relative standard deviations of 3.8％-12.8％.Results indicate that the magnetic metal-organic framework based dispersive micro-solid phase extraction is simple,rapid and high-loading for antibiotics enrichment from water,which further expand the practical application of metal-organic frameworks in sample pretreatment for environmental pollutant analysis.