Herein, an electrospun composite polyvinyl alcohol/zirconium–based metal–organic frameworks (PVA@UiO–66) nanofiber coating was prepared on the surface of stainless steel mesh (SSM) and then utilized as novel sorbent for the extraction of phthalate esters (PEs) in milk and water samples. Gas chromatography equipped with a flame ionization detector (GC–FID) was used for the quantitative determination of extracted analytes. The SSM coated with PVA@UiO–66 was used in a polypropylene syringe to fabricate the solid-phase extraction (SPE) device. The PVA@UiO–66 nanofiber coating was confirmed using X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy analysis (FT–IR), and field emission scanning electron microscopy (FESEM). The effective parameters of the extraction efficiency including volume and type of desorption solvent, sample volume, ionic strength, pH, extraction flow rate, and desorption flow rate were optimized. At the optimal extraction conditions, the calibration plots for phthalate esters were linear within the range of 0.05–100 ng mL−1 and, low detection limits (0.015–0.06 ng mL–1). Finally, this semi-automated SPE was used for the extraction and detection of phthalate esters (PEs) in milk and various environmental real water samples. The results showed good precision with acceptable and satisfactory extraction recovery values ranging from 89.5–99.2% and relative standard deviations (RSDs%) ranging from 4.5–6.9%.

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