RESUMO

This study describes a simple and sensitive voltammetric method for determining As (III) and As (V)concentrations in ìg.L-1. Electroactive As (III) is evaluated by direct analysis. As (V) is converted into As (III) using reduction solution; the new As (III) concentration, represents the total inorganic As in the analyzed sample. As (III) and total inorganic As determination showed a work potential peak at -0.68 V;As (V) concentration was determined by subtraction [total inorganic As As (III)]. Quantification and detection limits for As (III) were 0.22 and 0.08 ìg.L-1, respectively, for a deposition time of 180 s with the linear range from 1 to 5 ìg.L-1. Standard deviation for 1 to 5 ìg.L-1 arsenic concentration (n = 10) was 5%.The methodology was successfully applied for identifying and quantifying the inorganic arsenic in grape juices; and the accuracy was assessed by a recovery test on spiked samples, being 98.2% for As (III) and 96.4% for As (V). These results were compared with those from hydride generation atomic absorptions pectrometry analyses. The grape juice samples analyzed by voltammetric technique showed As (III) and As (V) concentrations ranging 51-71 ìg.L-1 and 34-60 ìg.L-1, respectively. (AU)

O presente estudo descreve um método voltamétrico simples e sensível para a determinação de As (III) e As (V), em μg.L-1. As (III) é determinado pela análise direta, e As (V) é convertido em As (III) por uma solução de redução. A nova concentração de As (III) representa a concentração de As inorgânico total na amostra em análise. As (V) foi determinado pela subtração do As inorgânico total e do As (III). Os limites de quantificação e detecção de As (III) foram, respectivamente, 0,22 e 0,08 μg.L-1 para o tempo de deposição de 180 s; a faixa linear foi de 1 a 5 μg.L-1 e desvio-padrão (n = 10) de 5%, em potencial de -0,68 V. A precisão foi verificada por meio de teste de recuperação em amostras fortificadas [de 98,2% para As (III) e de 96,4% para As (V)]. Estes resultados foram comparados com a análise feita por espectrometria de absorção atômica com geração de hidreto. O método voltamétrico foi aplicado na especiação do arsênio em amostras de sucos de uva contendo concentrações de 51 a 71 μg.L-1 de As (III) e 34 a 60 μg.L-1 de As (V). (AU)

Assuntos

RESUMO

This study describes a simple and sensitive voltammetric method for determining As (III) and As (V)concentrations in ìg.L-1. Electroactive As (III) is evaluated by direct analysis. As (V) is converted into As (III) using reduction solution; the new As (III) concentration, represents the total inorganic As in the analyzed sample. As (III) and total inorganic As determination showed a work potential peak at -0.68 V;As (V) concentration was determined by subtraction [total inorganic As – As (III)]. Quantification and detection limits for As (III) were 0.22 and 0.08 ìg.L-1, respectively, for a deposition time of 180 s with the linear range from 1 to 5 ìg.L-1. Standard deviation for 1 to 5 ìg.L-1 arsenic concentration (n = 10) was 5%.The methodology was successfully applied for identifying and quantifying the inorganic arsenic in grape juices; and the accuracy was assessed by a recovery test on spiked samples, being 98.2% for As (III) and 96.4% for As (V). These results were compared with those from hydride generation atomic absorptions pectrometry analyses. The grape juice samples analyzed by voltammetric technique showed As (III) and As (V) concentrations ranging 51-71 ìg.L-1 and 34-60 ìg.L-1, respectively.

Assuntos

RESUMO

Tuberculosis remains a major public health problem, especially in developing countries. Brazil presents the largest number of cases in Latin America and is among the 22 countries considered priorities by the World Health Organization (WHO). The Rio de Janeiro state has the largest number of cases registered in the country. The treatment of patients, commonly, makes use of the drugs isoniazid and rifampicin for six months. This study aimed to develop and validate an electroanalytical methodology, using the technique of differential pulse voltammetry for the determination of these drugs in the associated form, in order to evaluate the quality of medicines distributed in the state of Rio de Janeiro. The potential reduction for the isoniazid and rifampicin were -1.10 and -0.90 V. The developed and validated electroanalytical method presented a linear range of 0.25 to 1.25 mg/L to isoniazid, limits of detection and quantification of 0.05 and 0.14 mg/L, and recovery of 98.2 ± 0.4 percent; a tracking linear of 0.40 to 2.00 mg/L for rifampicin, with limits of detection and quantification of 0.07 and 0.19 mg/L and recovery of 95.8 ± 0.6 percent. Six lots of medicines from two pharmaceutical companies were analyzed. Only one of the samples showed unsatisfactory levels of rifampicin.

A tuberculose continua sendo um importante problema de saúde pública, especialmente em países em desenvolvimento. O Brasil apresenta o maior número de casos da América Latina, estando entre os 22 países considerados prioritários nas ações de controle da doença pela Organização Mundial da Saúde (OMS). No Brasil, o Rio de Janeiro é o estado com o maior número de casos registrados no país. O tratamento de doentes com tuberculose faz uso dos fármacos isoniazida e rifampicina durante seis meses. O presente trabalho objetivou desenvolver e validar metodologia eletroanalítica, utilizando a técnica de voltametria de pulso diferencial, para a determinação desses dois princípios ativos na forma associada e avaliar a qualidade dos medicamentos distribuídos no estado do Rio de Janeiro. Os potenciais de redução para a isoniazida e rifampicina foram respectivamente -1,10 e -0,90 V. O método eletroanalítico desenvolvido e validado apresentou para a isoniazida faixa linear de 0,25 a 1,25 mg/L, limites de detecção e quantificação de 0,05 e 0,14 mg/L e recuperação de 98,2 ± 0,4 por cento; para a rifampicina faixa linear de 0,40 a 2,00 mg/L, limites de detecção e quantificação de 0,07 e 0,19 mg/L e recuperação de 95,8 ± 0,6 por cento. Foram analisados 6 lotes de medicamentos de dois laboratórios farmacêuticos. Apenas uma das amostras apresentou teor de rifampicina insatisfatório.

Assuntos