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The present work introduced copper oxide nanoparticles as an efficient electrode modifier for sensitive adsorptive differential pulse voltammetric assaying of marbofloxacin (MRB) in pharmaceutical formulations and surface water samples. In the presence of sodium dodecyl sulphate (SDS) at pH 4.0, the marbofloxacin molecule was irreversibly oxidized at the electrode surface showing an anodic oxidation peak at 0.954 V. The electrode reaction mechanism was assumed as adsorption‐reaction controlled accompanied by the transferring of two electrons and proton exchange in agreement with the molecular orbital calculations performed on MRB molecule suggesting the oxidation of the amino group in the piperazinyl ring. At the optimized measuring conditions, the recorded peak heights were linearly correlated with the MRB concentration within the range from 6.67 to 360 ng mL−1, and the estimated LOD value was 2.2 ng mL−1. The integrated sensor showed a prolonged operational lifetime with good reproducibility of measurements. Based on the selectivity and sensitivity of the proposed method, MRB was successfully assayed in pharmaceutical formulations and surface water samples with mean average recoveries agreeable with the official method. [ABSTRACT FROM AUTHOR]

Three new potentiometric membrane sensors responsive to procainamide hydrochloride (PR) were constructed and their general performance characteristics were determined. The sensors were constructed from PR ion-association complexes with tetraphenylborate (NaTPB) (1), phosphomolybdic acid (PMA) (2) and phosphotungstic acid (PTA) (3) as exchange sites in a polyvinyl chloride (PVC) matrix. The sensors exhibited stable, rapid and near-Nernstian properties for PR at concentrations of $1\times 10^{{-2 }}$ – $4\times 10^{-6}$ , $1\times 10^{-2}- 5\times 10^{-6}$ , $1\times 10^{-2}$ – $6\times 10^{-6}$ M at 25 °C with cationic slopes of 58 ± 0.5, 57 ± 0.5 and 56 ± 0.5 (mV/decade) for sensor 1, 2 and 3 respectively. The response time of the sensors was 20s in the optimum pH range of 4-8. The sensors were used in steady state and flow injection mode (automated system). Method validation revealed the sensors have high selectivity, low detection limits, long life, wide dynamic ranges as well as high accuracy and precision. Direct determination of 5- $2000~\mu \text{g}$ /ml of PR in solution returned average recoveries of 98.5%, 99.0% and 98.5% and mean relative standard deviations of 1.6%, 1.6% and 1.8% at $200.0~\mu \text{g}$ /ml for sensor 1, 2 and 3 respectively. Further, detection of procainamide in spiked urine exhibited favorable relative standard deviation (1.60-1.76%) and high recovery (98.83-99.26%). The sensors were used as end-point indicators for titration of procainamide with NaTPB. [ABSTRACT FROM AUTHOR]