Functionalized MNPs were synthesized to serve as solidphase extraction sorbents for simultaneous enrichment and detection of endocrine disrupting compounds in milk samples with the aid of GC–MS. Analyte extraction and desorption were carried out quickly and the whole pretreatment process could be accomplished by simple vortex and ultrasonication with in 25 min. The applicability, accuracy, precision, sensitivity of the proposed method have been demonstrated based on SANCO/12571/2013 European Guidelines. LODs were below the MRLs set by the European Union for all compounds studied. Considering that Fe3O4@SiO2@C18 nanoparticles inherit the virtues of being easy-to-prepare, cost-effectivenessand ease of separation and dispersion, this protocol is believed tobe promising for the screening of the selected compounds in milkmatrices.