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Adsorptive Stripping Voltammetric method for Nimesulide (NIM) determination was developed. As a working electrode, glassy carbon electrode (GCE) modified with carbon black and Nafion (CB-Nafion GCE) was used. All measurements were carried out in 0.1 M acetate buffer (pH 4.6). Conducted experiments allowed to optimize differential pulse voltammetry (DPV) instrumental parameters: sampling and waiting time t s  = t w  = 10 ms, step potential E s  = 4 mV, and pulse amplitude ΔE = 50 mV. The best results were obtained for preconcentration potential and time equal to 400 mV and 20 s, respectively. Limit of detection was calculated and was equal to 0.14 µM for 20-s preconcentration time and 0.06 µM for 40-s preconcentration time. In order to prove the applicability of the developed method, concentration of nimesulide in pharmaceutical products was determined. Calculated recoveries were in the range 94–99%, which indicates that the method might be assumed as accurate. Coefficient of variation was equal to 5.0% (n = 7, NIM concentration 1 µM) Obtained results of NIM determination were in good agreement with the content declared by producers.

Nimesulide Determination on Carbon Black-Nafion Modified Glassy Carbon Electrode by Means of Adsorptive Stripping Voltammetry