Electroreduction and adsorption of cefixime was studied in phosphate buffer by cyclic voltammetry (CV), differential pulse cathodic adsorptive stripping voltammetry (DPCAdSV), and square-wave cathodic adsorptive stripping voltammetry (SWCAdSV) at hanging mercury drop electrode (HMDE). These fully validated sensitive and reproducible cathodic adsorptive stripping voltammetric procedures were applied for the trace determination of the bulk drug in pharmaceutical formulations and in human urine. The optimal experimental parameters were as follows: accumulation potential=-0.1 V (vs. Ag/AgCl, 3M KCl), accumulation time=50s, frequency=140 Hz, pulse amplitude=0.07 V, and scan increment=10 mV in phosphate buffer (pH 2.6). The first peak current showed a linear dependence with the drug concentration over the range of 50 ng ml(-1) to 25.6 μg ml(-1). The achieved limit of detection and limit of quantitation were 3.99 and 13.3 ng ml(-1) by SWCAdSV and 7.98 and 26.6 ng ml(-1) by DPCAdSV, respectively. The procedure was applied to assay the drug in tablets. Applicability was also tested in urine samples. Peak current was linear with the drug concentration in the range of 1 to 60 μg ml(-1) of the urine, and minimum detectability was found to be 12.6 ng ml(-1) by SWCAdSV and 58.4 ng ml(-1) by DPCAdSV.