In this study, electrospinning was used to synthesize the nanofibers from a blend of chitosan and polyvinyl alcohol (PVA) to remove acidic drugs from wastewater. Fibers with uniform morphology were obtained at voltage of 20 kV, flow rate of 0.2 mL/h, and collection distance of 10 cm. The chemical and physical properties of the produced nanofibers were investigated utilizing a variety of equipment, including SEM, FTIR, XRD, and TGA-DSC. The nanofibers contain active hydroxyl and amino functional groups with an average diameter of 380 nm, according to the characterization results of FTIR and SEM. From the XRD and TGA-DSC analysis, the nanofibers were found to be amorphous and thermally stable at 200 °C. A thermal treatment to the nanofibers was done to reduce the water solubility of the fibers prior to their application for the adsorption of acidic drugs from water systems. Using the ultra-pure water, maximum removal capacities (qm) were calculated from Langmuir isotherm and were found to be 27.85, 1666.66, 166.6, and 1250 mg/g for acetyl salicylic acid, naproxen, fenoprofen, and diclofenac, respectively.