<p>In this study, an innovative hydrophobic membrane was developed using electrospinning to integrate zeolitic imidazolate framework-67 (ZIF-67) and polyacrylonitrile (PAN) nanofibers (PAN/ZIF-67 NFs). This research highlights the significance of an in situ fabrication process, eliminating the need for pre-seeding or surface modification. By incorporating Co²⁺ into a PAN solution in N,N-dimethylformamide (DMF), Co²⁺ ions interact with the nitrile (N≡C<i>–</i>) groups of the polymer, facilitating the subsequent formation of ZIF-67 nanoparticles upon adding 2-methylimidazole. This in situ synthesis method results in significantly thinner nanofibers compared to pristine PAN due to the uniform dispersion and nucleation of ZIF-67 on the polymer chains. The reduced fiber diameter decreases membrane porosity, potentially enhancing filtration and mechanical properties. The PAN/ZIF-67 membrane effectively removes acetaminophen (ACE) illustrating 89.9% efficiency within 20 min. Similarly, ibuprofen (IBP) removal is most efficient, with a 96.03% efficiency in the same timeframe. Mechanistic insights reveal that π-π stacking interactions, H-bonding, and physical penetration are the dominant factors contributing to adsorption, facilitated by the large active surface area and pore volume of the PAN/ZIF-67 membrane. Thus, the PAN/ZIF-67 membrane stands out as a promising candidate for superior adsorption applications.</p> Graphical abstract <p></p>