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Sample preparation methods with high accuracy and matrix resistance will benefit the quick analysis of desired analytes in an intricate matrix, such as the monitoring of drug samples in biofluids. Herein, an electrospun composite, consisting of polyfam and a Co-metal organic framework- 74, was developed as a novel sorbent for the high-throughput solid-phase micro-extraction of certain anti-cancer drugs (sorafenib, dasatinib, and erlotinib hydrochloride) from wastewater and biological samples before high-performance liquid chromatography- ultraviolet analysis (HPLC-UV). The synthesis of the resulting composite nanofibers was confirmed using the techniques of Fourier transform-infrared spectroscopy, field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), and powder X-ray diffraction (XRD). FESEM images illustrated irregular and bead-free nanofibers with a …