Abstract

Nitroxoline has been reduced at the mercury electrode in buffered solutions (pH 2−11) in two irreversible cathodic steps. The first step was attributed to reduction of –NO 2 group to the hydroxylamine stage and the second one to reduction-saturation of the C=N double bond. DC-polarographic and various adsorptive stripping voltammetric methods were developed for determination of nitroxoline in bulk form. Limits of quantitation of 1.02 × 10 −6, 3.05 × 10 −8, 9.01 × 10 −9, and 9.12 × 10 −10 M nitroxoline were achieved by means of the developed DC-polarography, differential-pulse-, linear-sweep-, and square-wave-adsorptive cathodic stripping voltammetric methods, respectively. All these electroanalytical methods were successfully applied for determination of nitroxoline in its Nibiol ® tablets. While only the developed adsorptive stripping voltammetry methods were successfully applied for determination of the drug in spiked human serum and for pharmacokinetic studies in real human plasma. The analysis was carried out without interference from common excipients and without the necessity for prior extraction or interaction with any reagent during the analysis.

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