Cathodic adsorptive stripping voltammetric determination of nalidixic acid in pharmaceuticals, human urine and serum

Abstract

The quinolone antibacterial agent nalidixic acid (NAL) was studied by cyclic voltammetry (CV) and cathodic adsorptive stripping voltammetry (CASV). A sensitive method is described for the determination of NAL in its pure form, dosage forms and biological fluids. Controlled adsorptive accumulation of NAL on a hanging mercury drop electrode provides the basis for the direct stripping measurement of that compound in the nanomolar concentration level. Different variables were studied and optimized. The proposed method depends upon the voltammetric activity of NAL in Britton–Robinson buffer, whereby a well-defined cathodic peak is produced at pH 5.0 in presence of NO 3 −. The calibration graph to determine NAL was linear in the range 7.4×10 −8–2.5×10 −5 M by CASV. CAS voltammetry has been proved to be advantageous over a liquid chromatographic (LC) technique, allowing to detection limit signal to noise ratio, (s/n=3) of 0.766 ng ml −1 (3.3×10 −9 M) NAL to be reached. The relative standard deviation ( n=5) was 5.2% at concentration level of 1.0×10 −7 M NAL. The degree of interference from coexisting metal ions on the CASV signal for NAL was evaluated. The method was applied to two different commercial pharmaceutical products (Negram tablets and suspension) with very good recoveries. It was also shown that the method was successfully applied to the determination of NAL in human urine and blood serum. Mean recoveries were 98.8±0.3 and 98.9±0.41%, respectively.