Multi-wall carbon nanotube poly L-Lysine (MWCNTs-PLL) material was effectively synthesized in this study. UV-Vis spectrum and Fourier transform infrared spectroscopy were used to determine the structure of nanoparticles. The electrochemical characteristics of glassy carbon electrodes (GCE) were examined after the MWCNTs-PLL material with nanosized particles was dropped onto its surface to create MWCNTs-PLL/GCE. Employing electrodes, Paracetamol (PAR) and Ibuprofen (IBU) were examined via applying CV and DP-ASV techniques. In comparison to employing the bare GCE, the modified MWCNTs-PLL/GCE electrode showed good responsiveness toward PAR and IBU applying the DP-ASV technique, with limits of detection of 0.40 for PAR and 0.34 μM for IBU. The linear concentrations ranged from 1.0 to 210 μM. Factors such as Na+, SO42-, CO32-, K+, Ca2+, Cl-, Mg2+, NH4+, NO3- ions, uric acid, oxalate and AA, did not interfere during the modified electrode’s operation. Note that these analytical processes for the PAR and IBU in practical sample solutions are more dependable than the HPLC tool.