Functionalized MNPs were synthesized to serve as solid-phaseextraction sorbents for simultaneous enrichment and detection ofendocrine disrupting compounds in milk samples with the aid ofGC–MS. Analyte extraction and desorption were carried out quicklyand the whole pretreatment process could be accomplished bysimple vortex and ultrasonication within 25 min. The applicabil-ity, accuracy, precision, sensitivity of the proposed method havebeen demonstrated based on SANCO/12571/2013 European Guide-lines. LODs were below the MRLs set by the European Union for allcompounds studied. Considering that Fe3O4@SiO2@C18 nanoparti-cles 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.