Rapid and effective sample cleanup based on graphene oxide-encapsulated core–shell magnetic microspheres for determination of fifteen trace environmental phenols in seafood by liquid chromatography–tandem mass spectrometry

• Novel graphene oxide-encapsulated core-shell magnetic microspheres (GOE-CS-MM) were fabricated by a self-assemble approach.
• The as-prepared material GOE-CS-MM exhibited excellent cleanup efficiency and could availably reduce the matrix effect.
• The cleanup mechanisms refer to π–π stacking interaction and hydrogen bond.
• The developed MSPE–LC–MS/MS method was simple, fast, sensitive and accurate.

In this study, graphene oxide-encapsulated core–shell magnetic microspheres (GOE-CS-MM) were fabricated by a self-assemble approach between positive charged poly(diallyldimethylammonium) chloride (PDDA)-modified Fe3O4@SiO2 and negative charged GO sheets via electrostatic interaction. The as-prepared GOE-CS-MM was carefully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer analysis (VSM), and X-ray photoelectron spectroscopy (XPS), and was used as a cleanup adsorbent in magnetic solid-phase extraction (MSPE) for determination of 15 trace-level environmental phenols in seafood coupled to liquid chromatography–tandem mass spectrometry (LC–MS/MS). The obtained results showed that the GOE-CS-MM exhibited excellent cleanup efficiency and could availably reduce the matrix effect. The cleanup mechanisms were investigated and referred to π–π stacking interaction and hydrogen bond between GOE-CS-MM and impurities in the extracts. Moreover, the extraction and cleanup conditions of GOE-CS-MM toward phenols were optimized in detail. Under the optimized conditions, the limits of detection (LODs) were found to be 0.003–0.06 μg kg−1, and satisfactory recovery values of 84.8–103.1% were obtained for the tested seafood samples. It was confirmed that the developed method is simple, fast, sensitive, and accurate for the determination of 15 trace environmental phenols in seafood samples.

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