Nifedipine is a calcium-channel antagonist drug used in the management of angina pectoris and hypertension through inhibition of calcium influx. A fully validated sensitive cathodic adsorptive stripping square-wave voltammetry procedure was optimized for the determination of the drug at trace levels. The procedure was based on the reduction of the nitrophenyl group after the interfacial accumulation of the drug onto a hanging mercury drop electrode in Britton-Robinson buffer of pH 11.0. The optimal conditions of the procedure were found to be: accumulation potential=-0.9 V vs. Ag/AgCl/KCl(s)), accumulation time=30 s, scan increment=10 mV, pulse amplitude=50 mV and frequency=120 Hz. Under these conditions, a well-defined peak was obtained; its peak current showed a linear dependence on drug concentration in the range of 2x10(-9)-2x10(-7) mol L(-1) bulk nifedipine. The mean recoveries based on eight replicate measurements for 1x10(-8) and 5x10(-8) mol L(-1) bulk nifedipine solutions were 98.46+/-0.86% and 98.23+/-0.92%, respectively. A detection limit of 3.42x10(-10) mol L(-1) bulk nifedipine was achieved. The procedure was successfully applied for assay of the drug in tablets and spiked human serum with mean recoveries of 101.95+/-1.42% and 98.70+/-0.63%, respectively. The limit of detection of the drug in spiked human serum was found to be 3.90x10(-10) mol L(-1).
A rapid and sensitive square-wave voltammetric procedure was optimized for the determination of dipyridamole after its adsorption preconcentration onto a hanging mercury drop electrode. The peak current of the first of the two peaks developed for this drug in Britton-Robinson buffer at pH 8.0 has been considered for the present analytical study. An accumulation potential of -1.0 V versus Ag/AgCl/KCl(s), pulse amplitude a =100 mV, scan increment Delta E =10 mV, and frequency f =120 Hz were the optimal experimental parameters. Dipyridamole can be determined in the concentration range of 9.0 x 10(-9) to 5.0 x 10(-6) M using accumulation times of 30-300 s. A detection limit of 4.0 x 10(-11) M was achieved after a 300 s accumulation time. Applicability to serum samples was illustrated. The average recoveries for dipyridamole spiked to serum at 0.25-4.50 micro g ml(-1) were 96.0-102.0%, and the higher standard deviation was 2.9%. A detection limit of 0.06 micro g mL(-1) of serum was obtained.
The electrochemical reduction of the anti-inflammatory drug ketoprofen was studied in a Britton-Robinson (B-R.) buffer series of pH 211 using dc-polarography, cyclic voltammetry, and coulometry techniques. The electrode reaction pathway of the drug at the dropping mercury electrode was proposed and discussed. A new adsorptive cathodic stripping square-wave voltammetric procedure was optimized for the assay of bulk drug in a B-R. buffer of pH 2.0. The peak current was linear with the drug concentration over the ranges 2 × 109 to 2 × 107 M of the bulk drug, using a 60 s accumulation time period at 0.6 V (vs. Ag/AgCl/KCls). The percentage recovery of the bulk drug was 99.57 ± 0.54 and a detection limit of 0.10 ng mL1 was achieved. The proposed procedure was successfully applied for the assay of ketoprofen in pharmaceutical formulation (Ketofan®) and human plasma. The percentage recoveries were 99.66 ± 0.47 and 101.76 ± 0.64 in pharmaceutical formulation and human plasma, respectively. A detection limit of 0.14 ng mL1 plasma was achieved which was below that reported in literature using the different analytical techniques.Key words: ketoprofen (Ketofan®) determination, polarography, cyclic voltammetry, adsorptive cathodic stripping square-wave voltammetry, human plasma.
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