Fe3O4@SiO2@UiO-66　core-shell　magnetic　microspheres　were　synthesized　and　characterized　by　transmission　electron　microscopy,　scanning　electron　microscopy,　X-ray　diffraction,　Fourier　transform　infrared　spectrometry,　vibrating　sample　magnetometry,　nitrogen　adsorption　porosimetry　and　zeta　potential　analyzer.　The　synthesized　Fe3O4@SiO2@UiO-66　microspheres　were　first　used　for　magnetic　solid-phase　extraction　(MSPE)　of　domoic　acid　(DA)　in　shellfish　samples.　Combined　with　high　performance　liquid　chromatography-tandem　mass　spectrometry　(HPLC-MS/MS),　a　fast,　simple　and　sensitive　method　for　the　determination　of　DA　was　established　successfully.　Under　the　optimized　conditions,　the　developed　method　showed　short　analysis　time,　good　linearity　(r(2)　=　0.9990),　low　limit　of　detection　(1.45　pg　mL(-1);　S/N　=　3:1),　low　limit　of　quantification　(4.82　pg　mL(-1);　S/N　=　10:1),　and　good　extraction　repeatability　(RSD　＜=　5.0%;　n　=　5).　Real　shellfish　samples　were　processed　using　the　developed　method,　and　trace　level　of　DA　was　detected.　The　results　demonstrate　that　Fe3O4@SiO2@UiO-66　core-shell　magnetic　microspheres　are　the　promising　sorbents　for　rapid　and　efficient　extraction　of　polar　analytes　from　complex　biological　samples.　(C)　2015　Elsevier　B.V.　All　rights　reserved.