Griseofulvin is an antifungal antibiotic used to treat various pathogenic mycotic diseases. The voltammetric behavior of griseofulvin at a hanging mercury drop electrode in Britton-Robinson buffers of pH 2 -11.5 was studied and discussed. A fully validated sensitive square-wave adsorptive cathodic stripping voltammetric procedure was described for direct determination of bulk griseofulvin substance. The procedure was based on the reduction of the .C5 5O double bond of griseofulvin molecule following its preconcentration onto a hanging mercury drop electrode in a Britton-Robinson buffer of pH 10. Limits of detection (LOD) and quantitation (LOQ) of 5.8 Â 10 210 M and 1.93 Â 10 29 M bulk griseofulvin were achieved, respectively. The proposed stripping voltammetric procedure was successfully applied to assay griseofulvin in tablets and in spiked human serum and urine samples. LOD of 8.65 Â 10 210 M and 6.6 Â 10 29 M and LOQ of 2.88 Â 10 29 M and 2.2 Â 10 28 M griseofulvin in spiked human serum and urine samples, respectively, were achieved.