Determinação simultânea de aspirina e ácido ascórbico em medicamentos usando análise por injeção em fluxo com detecção amperométrica
Ano de defesa: | 2011 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Uberlândia
BR Programa de Pós-graduação em Química Ciências Exatas e da Terra UFU |
Programa de Pós-Graduação: |
Não Informado pela instituição
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Departamento: |
Não Informado pela instituição
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País: |
Não Informado pela instituição
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Palavras-chave em Português: | |
Link de acesso: | https://repositorio.ufu.br/handle/123456789/17349 https://doi.org/10.14393/ufu.di.2011.140 |
Resumo: | The present study investigated a simple, low-cost and, high analytical frequency method for simultaneous determination of ascorbic acid (AA) and acetylsalicylic acid (ASA) in pharmaceutical formulations. The methodology is based on flow injection analysis with multiple-pulse amperometric detection (FIA-MPA) using boron-doped diamond (BDD) as working electrode. The oxidation current peak of AA reaches a maximum near to 0.9 V and for salicylic acid (hydrolyzed AAS) near to 1.35 V (acetic acid/acetate buffer; pH = 4,7). The strategy used for simultaneous determination of the two compounds by FIA-MPA was the following: (1) +0.90 V/50 ms: AA oxidation and its selective quantification; (2) +1.35 V/50 ms: Oxidation of both AA and AS compounds. AS can be then quantified by subtraction of the currents obtained from both potential pulses (using a correction factor), because the oxidation currents of AA are not the same at both potential pulses. The current from the oxidation of AS is obtained from the following equations: factor = IAA +1.35 V/IAA +0.9 V IAS = I1.35 V (I0.90 V x factor) (3) +0.00 V/300 ms: applied to avoid contamination of the working electrode surface. The proposed method presented linear range response between 10 and 90 μmol L-1 and between 16 and 200 μmol L-1 for AA and AS, respectively. The repeatability study (n = 10) demonstrated that the method is stable with the RSD equal to 0.5 %. The analytical frequency was estimated to be 125 injections per hour and the limit of detection of 174 and 164 nmol L-1 for AA and AAS, respectively. Results were compared to those obtained by an HPLC method and statistical analysis was used to compare these results. At a 95% confidence level it was verified that both methods showed similar results (Student s t-test) and equivalent accuracies (F test). Additional studies for simultaneous determination of AA and AAS were also carried out using Batch Injection Analysis (BIA) and Square Wave Voltammetry (SWV). |