A novel, simple and sensitive adsorptive stripping voltammetry method was developed for simultaneous determination of Cd and Zn using N-Nitrozo-N-phenylhydroxylamine (Cupferron) as a selective complexing agent. Cadmium and zinc metals gave peaks that were distinctly separated by 450–1200 mV, allowing their determination over a wide range of concentrations. The influence of pH and the nature of supporting electrolytes, concentration of ligand, preconcentration time and applied potential were investigated. The detection limits were 0.058 ng/mL for Zn and 0.092 ng/mL for Cd, and the RSD at a concentration level of 50 ppb, were 1.8–2.1% for both zinc and cadmium, respectively. The method was applied to the determination of cadmium and zinc in blood, drug, food and water samples with the satisfactory results.
