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An electrospun composite polyacrylonitrile/iron (III)/Mg-based metal–organic framework 88B (PAN/Fe/Mg-MIL-88B) was prepared, and then utilized as a viable sorbent for the simultaneous determination of five phthalate esters in store-bought bottled mineral water and orange juice, urine, plasma, and two different types of cream and lipstick applying spin column micro solid-phase extraction (SC-μSPE) method. The synthesis of the electrospun nanofibers was surveyed using energy-dispersive X-ray spectroscopy, X-ray diffraction analysis and Fourier transform infrared spectroscopy, while the morphology of the composite was investigated using field emission scanning electron microscopy. The presence of Fe/Mg-MIL-88B with high quantity of functional groups and porous structure in the polymer matrix endows the PAN nanofibers with high extraction efficiency. The effect of MOF% in the composite nanofibers …