The polarographic and voltammetric behaviour of mitoxantrone has been studied. A well-defined linear sweep voltammetric peak was found at -0.83 V (vs. SCE) in HEPES buffer (50 mmol/L, pH 7.0). The experimental results prove that the reduction peak of mitoxantrone has adsorptive characteristics. A single-sweep oscillopolarographic method was developed for the determination of mitoxantrone in human serum and urine. The peak current (iP) is proportional to concentration in the range 5 × 10−7-5 × 10−5mol/L.