Penicillins can be electrochemically oxidized on gold electrodes in the presence of a catalytic surface oxide. Although oxidation can occur throughout a wide range of pH values, an acetate buffer solvent was selected to maximize the sensitivity and stability. Several amperometric waveforms were tested for penicillin detection using flow injection analysis. The use of pulsed amperometric detection (PAD) allowed the penicillins to be monitored either directly or indirectly depending on the specified waveform. Direct detection using standard PAD proved to be the optimal detection method, featuring excellent reproducibility and detectability to 4 X lo-' M for penicillin G.