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Analytical determination of nimesulide and ofloxacin in pharmaceutical preparations using square-wave voltammetry
Authors:Francisco W. P. Ribeiro  Thisiania R. V. Soares  Sameque do N. Oliveira  Luisa C. Melo  Janete E. Soares  Helena Becker  Djenaine De Souza  Pedro de Lima-Neto  Adriana N. Correia
Affiliation:1. Departamento de Química Analítica e Físico-Química, Centro de Ciências, Universidade Federal do Ceará, Bloco 940 Campus do Pici, 60455-970, Fortaleza — CE, Brazil
2. Departamento de Farmácia, Faculdade de Farmácia, Odontologia e Enfermagem, Universidade Federal do Ceará, Rua Capit?o Francisco Pedro, 1210 Rodolfo Teófilo, 60430-370, Fortaleza — CE, Brazil
3. Campus de Patos de Minas — Instituto de Química, Universidade Federal de Uberlandia, Av. Getúlio Vargas, 230 Centro, CEP 38700-126, Patos de Minas — MG, Brazil
Abstract: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.
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