Fe3O4@MOF core–shell magnetic microspheres for magnetic solid-phase extraction of polychlorinated biphenyls from environmental water samples

• Fe3O4@MOF core–shell magnetic microspheres were prepared as magnetic SPE sorbent.
• Box–Behnken design was used to optimize extraction conditions through RSM.
• Fe3O4@MOF core–shell magnetic microsphere achieved high extraction efficiency.

Fe3O4@MIL-100 core–shell magnetic microspheres were, for the first time, used as the sorbent for the magnetic solid-phase extraction (MSPE) of polychlorinated biphenyls at trace levels in environmental water samples. GC coupled with tandem MS was used for sample quantification and detection. The Box–Behnken design was used to determine the optimum extraction parameters influencing extraction efficiency through response surface methodology. Under the optimized conditions, the developed method showed good linearity within the range of 5–4000 ng L−1, low limits of detection (1.07–1.57 ng L−1; signal-to-noise ratio = 3:1), and good extraction repeatability (relative standard deviation < 12%; n = 5). Environmental samples collected from the Yellow River, local lake, wastewater, and snow water were processed using the developed method. The results demonstrated that the Fe3O4@MOF core–shell magnetic microspheres are promising sorbents in the MSPE of aromatic pollutants from environmental water samples.