Solid microparticles of local anesthetics benzocaine, cinchocaine, lidocaine and procaine, and the antithusic codeine were mechanically immobilized on the surface of the paraffin impregnated graphite electrode and investigated by square-wave and cyclic voltammetry in order to develop a method for their qualitative determination. The measurements were performed in the pH range between 1 and 9. The square-wave frequency and amplitude were changed between 100 and 1000 Hz, and from 15 to 85 mV, respectively. The scan rate in cyclic voltammetry was 1 V/s.