Abstract: In this study, Fe3O4@Si O2@MIP core- shell nanocomposite was synthesized by surface molecular imprinting technique. It had an ability of selective extraction and detection of tetracycline antibiotics. The magnetic solid-phase extraction combined with high performance liquid chromatography(MSPE-HPLC) detects three kinds of antibiotic residues simultaneously. The magnetic Fe3O4@Si O2@MIP core-shell nanocomposites was characterized by scanning electron microscopy( SEM), transmission electron microscopy( TEM) and Fourier transform infrared( FT- IR) analysis. The result showed that the limit of detection of tetracycline,oxytetracycline and chlortetracycline was 9.61,7.84 and 11.93 μg/kg,respectively;the maximum adsorption capacity of magnetic Fe3O4@Si O2@MIP molecularly imprinted polymers was obtained at 56.28 mg/g,its recoveries ranging from 93.71% to 100.88% were obtained with relative standard deviations in the range of 1.54%~7.44%.Compared with Fe3O4@Si O2@NIP,the selective adsorption of Fe3O4@Si O2@MIP was more capable.