The electroreduction behaviour and determination of cefoperazone using a hanging mercury drop electrode were investigated. Cyclic voltammograms of cefoperazone recorded in universal Britton-Robinson buffers pH 3–6 exhibited a single irreversible cathodic peak. The process was adsorption-controlled. Britton-Robinson buffer 0.04？M pH 4.0 was selected as a supporting electrolyte for quantitative purposes by differential pulse and square wave adsorptive cathodic stripping voltammetry. The experimental voltammetric conditions were optimized using Central Composite Face design. A reduction wave was seen in the range from ？0.7 to ？0.8？V. These voltammetric techniques were successfully validated as per ICH guidelines and applied for the determination of cefoperazone in its single and sulbactam containing powders for injection and statistically comparable to USP-HPLC. They were further extended to determine cefoperazone in spiked human urine with no matrix effect. 1. Introduction Cefoperazone is a third-generation cephalosporin antibiotic effective in treating Pseudomonas aeruginosa infections, which are otherwise resistant to other antibiotics. Chemically, it is described as (6R,7R)-7-[(2R)-2-{[(4-ethyl-2,3-dioxopiperazin-1-yl)carbonyl]amino}-2-(4-hydroxyphenyl)acetamido]-3-{[(1-methyl-1H-1,2,3,4-tetrazol-5-yl)sulfanyl]methyl}-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid. Its good activity, particularly against Enterobacteriaceae and Bacteroides spp., has been enhanced in the presence of the beta-lactamase inhibitor sulbactam. It is given intramuscularly or intravenously as the sodium salt. Although the drug is mainly excreted in the bile, urinary excretion primarily by glomerular filtration accounts for up to 30% of a dose unchanged within 12 to 24 hours [1]. In the literature, the determination of cefoperazone has been achieved by high performance liquid chromatography (HPLC) [2–6], thin layer chromatography [7], electrophoresis [8], UV spectrophotometry [9–14], spectrofluorimetry [15, 16], colorimetry, and atomic absorption spectrometry [17]. Although voltammetric techniques were also used for this purpose [18–21], the electroanalytical mechanism of cefoperazone was not clearly presented as well as its determination in the presence of sulbactam not being investigated. This work aimed at presenting a validated, simple, and sensitive adsorptive stripping voltammetric procedure for the quantification of cefoperazone in pharmaceutical formulations and spiked human urine, in particular overcoming the above-mentioned drawbacks in voltammetrically
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