Analytical determination of nimesulide and ofloxacin in pharmaceutical preparations using square-wave voltammetry

• Published in: Journal of analytical chemistry (New York, N.Y.) Vol. 69; no. 1; pp. 62 - 71
• Main Authors: Ribeiro, Francisco W. P., Soares, Thisiania R. V., do N. Oliveira, Sameque, Melo, Luisa C., Soares, Janete E., Becker, Helena, De Souza, Djenaine, de Lima-Neto, Pedro, Correia, Adriana N.
• Format: Journal Article
• Language: English
• Published: Boston Springer US 2014; Springer
• Subjects: Analytical Chemistry; Chemistry; Chemistry and Materials Science; Dosage and administration; Electrochemical reactions; Ofloxacin; Voltammetry; Brazil; ofloxacin; electrochemical behaviour; square-wave voltammetry; nimesulide; pharmaceutical formulations
• ISSN: 1061-9348; 1608-3199
• DOI: 10.1134/S1061934814010079

The electrochemical behaviour and analytical detection procedure for nimesulide ( NIM ) and ofloxacin ( OFX ) and their assay in commercial formulations were evaluated using square-wave voltammetry ( SWV ) combined with a hanging mercury drop electrode ( HMDE ). All experimental and voltammetric conditions were previously optimized to obtain the best analytical signal in terms of intensities and profile of the reduction peaks. For NIM, the peak currents were related to the one-electron reduction of a nitro group to a stable radical anion, which is followed by a one-electron transfer and a protonation step with a consequent formation of a nitrosoanion. The voltammetric results indicated that the mechanism of OFX involved the transfer of two electrons and two protons in a totally irreversible reduction related to the conversion of a ketone group to an alcohol group. Analytical parameters such as linearity range, equations of the analytical curves, correlation coefficients, detection and quantification limits, recovery efficiency, and relative standard deviation for repeatability and reproducibility experiments were compared to similar results obtained by the use of UV-Vis spectrophotometry, and the results showed that the voltammetric procedure using HMDE is suitable to determine pharmaceutical compounds in complex samples. The applicability of the proposed procedure was tested on pharmaceutical formulations of NIM and OFX by observing the stability, specificity, recovery and precision of the procedure in tablets, oral solution and ophthalmic solution.