Gold disk microelectrodes (AuMEs, 50 μm O) have been used for the determination of the fungicide disulfiram (DSF) at low concentration levels by differential pulse adsorptive stripping voltammetry (dp-AdSV). The AuMEs were fabricated in the laboratory and characterized by scanning electron microscopy and cyclic voltammetry. The AuME was pretreated daily by polishing with 3-μm diamond powder for 60 s, and by applying successively potentials of −0.4, −0.8, −1.0, −1.2 and −1.5 V for 30 s each in 0.1 mol L−1 H2PO4−/HPO42− (pH 6.0). In between measurements, the application of a potential of −1.5 V for 30 s was only necessary. The DSF adsorption on the AuME surface allows its determination at trace levels by dp-AdSV using low supporting electrolyte concentrations (3.0 mmol L−1) with an accumulation time of 120 s, a pulse amplitude of 50 mV, and a scan rate of 50 mV s−1. A detection limit of 6.3×10−8 mol L−1 and a RSD of 1.3% at a 5.0×10−7 mol L−1 DSF concentration level (n=10) were obtained with a two-electrode system and no stirring during the deposition step. The effect of the presence of several potential interferences on the DSF stripping signal has been tested. The developed method has been applied to the determination of DSF in spiked pea seeds with good results.