designa b s t r a c tA rapid magnetic solid-phase extraction (MSPE) is proposed based on C18-functionalized magnetic silicananoparticles as sorbents, for the determination of endocrine disruptors – 20 organochlorine pesticidesand 6 polychlorinated biphenyls – in milk samples. Magnetic nanoparticles are characterized by sev-eral techniques, such as Scanning Electron Microscopy, X-Ray diffraction, Brunauer–Emmett–Teller andFourier transform-infrared. The MSPE is performed by dispersion of the Fe3O4@SiO2@C18 nanoparticlesin milk samples with sonication, after protein precipitation. Then, the sorbent is collected by apply-ing an external magnetic field and the analytes are desorbed by n-hexane. Several parameters affectingthe extraction efficiency of target analytes by the magnetic nanoparticles are investigated, includingwashing and elution solvents, amount of sorbents, time of extraction and elution, sample and elutionsolvent volume. The proposed method is optimized by means of experimental design and response sur-face methodology. When coupled with gas chromatography–mass spectrometry detection and underoptimum extraction conditions, average recoveries of target analytes are found to be in the range of 79%to 116%. The proposed MSPE–GC–MS analytical method has a linear calibration curve for all target ana-lytes with coefficients of determination to range from 0.9950 to 0.9999. The limits of quantification arefound to be between 0.2 and 1 g/L ensuring compliance with the maximum residue limits establishedby European Commission and Codex Alimentarius, for OCPs and PCBs residues in milk. The proposedmethod is applied to the determination of target analytes in milk samples from local markets.