Granisetron showed one well-defined reduction peak at Hanging Mercury Drop Electrode (HMDE) in the potential range from −1.3 to −1.5 V due to reduction of C=N bond. Solid-phase extraction technique was employed for extraction of Granisetron from spiked human plasma. Granisetron showed peak current enhancement of 4.45% at square-wave voltammetry and 5.33% at cyclic voltammetry as compared with the non stripping techniques. The proposed voltammetric method allowed quantification of Granisetron in pharmaceutical formulation over the target concentration range of 50–200 ng/mL with detection limit 13.63 ng/mL, whereas in human plasma 50–225 ng/mL with detection limit 11.75 ng/mL. Keywords: Granisetron, Human plasma, Solid-phase extraction, Pharmaceutical formulation, Voltammetry, Hanging mercury drop electrode