For the construction of the sensor, three different carbon black (CB) materials (VULCAN XC72R, BLACK PEARLS 4750 and CB N220) were explored as modifying nanomaterial. Firstly, the electrochemical activity of the each SPE modified was compared by cyclic voltammetry and electrochemical impedance spectroscopy technique, using [Fe(CN)6]3−/4− as redox couple. After demonstrating that electrodes modified with different types of CB were characterized by improved electrochemical performances when compared with bare electrodes, and among them, electrodes modified with CB BP4750 is characterised by slightly better electrochemical properties, this type of electrode was used for the development of the analytical method. By applying SWV technique in 0.2 mol L−1 phosphate buffer (pH 3.0), the obtained analytical curves for ACP and LVF were found linearly from 4.0 to 80.0 μmol L−1 and from 0.90 to 70.0 μmol L−1 with limit of detection of 2.6 μmol L−1 and 0.42 μmol L−1 for ACP and LVF, respectively. Finally, the quantification of these drugs in river water was evaluated using the new here‐proposed sensor by recovery method in spiked samples, obtaining satisfactory recovery values. The results achieved demonstrated that the developed analytical tool is of great analytical interest being easy to use, cost‐effective, miniaturized, and thus suitable for low cost on site analysis.