Development and validation of an electroanalytical methodology for determination of isoniazid and rifampicin content in pharmaceutical formulations

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%; 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%. 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%; 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%. Foram analisados 6 lotes de medicamentos de dois laboratórios farmacêuticos. Apenas uma das amostras apresentou teor de rifampicina insatisfatório

Tamanho de amostra para estimar coeficientes de correlação linear de Pearson em espécies de crotalária

The objective of this work was to determine the necessary sample size to estimate Pearson’s linear correlation coefficients of four species of crotalaria at precision levels. The experiment was carried out with Crotalaria juncea, Crotalaria spectabilis, Crotalaria breviflora, and Crotalaria ochroleuca, during the 2014/2015 crop year. Eight crotalaria traits were evaluated in 1,000 randomly collected pods per species. For each species, the correlation coefficients were estimated for the 28 pairs of traits, and the sample size necessary to estimate the correlation coefficients was determined at four precision levels [0.10, 0.20, 0.30, and 0.40 amplitudes of the 95% (CI95%) confidence interval] by resampling with replacement. The sample size varies between crotalaria species and, especially, between pairs of traits, as a function of the magnitude of the correlation coefficient. At a certain precision level, the smallest sample size is required to estimate the correlation coefficients between highly correlated traits and vice-versa. To estimate the correlation coefficients with CI95% of 0.20, 10 to 440 pods are required, depending on the species, pairs of traits, and magnitude of the correlation coefficient.O objetivo deste trabalho foi determinar o tamanho de amostra necessário para estimar os coeficientes de correlação linear de Pearson em quatro espécies de crotalária, em níveis de precisão. O experimento foi realizado com Crotalaria juncea, Crotalaria spectabilis, Crotalaria breviflora e Crotalaria ochroleuca, no ano agrícola 2014/2015. Oito características da crotalária foram avaliadas em 1.000 vagens coletadas aleatoriamente por espécie. Para cada espécie, estimaram-se os coeficientes de correlação para os 28 pares de características e determinou-se o tamanho de amostra necessário para a estimação dos coeficientes de correlação, em quatro níveis de precisão [amplitudes do intervalo de confiança de 95% (CI95%) de 0,10, 0,20, 0,30 e 0,40] por reamostragem com reposição. O tamanho de amostra varia entre as espécies de crotalária e, principalmente, entre os pares de características, em função da magnitude do coeficiente de correlação. Em determinado nível de precisão, o menor tamanho de amostra é necessário para a estimação de coeficientes de correlação de alta magnitude e vice-versa. Para estimar coeficientes de correlação com CI95% de 0,20, são necessárias de 10 a 440 vagens, a depender da espécie, dos pares de características e da magnitude do coeficiente de correlação

Clinical and Nutritional characterization of patients with massive intestinal resection in Ribeirão Preto, SP, Brazil

Background: Short bowel syndrome (SBS) is a clinical situation due to extensive intestinal resection or dysfunction of the absorptive system of the small intestine. When these patints are not submitted to nutritional therapy their maximum survival is six months. In Brazil there are few reference centers for the treatment and follow-up of these patients and information about their characterization is scarce. Objective: To describe enterectomized patients attended during the period from 1996 to 2007. Methods: All medical records of the patients attended at the Nutrology service of HCFMRP-USP were analyzed retrospectively. Data were collected and analyzed descriptively using the contingency test and the Wilcoxon- Mann-Whitney test for independent samples. Results: Thirty-eight patients with a mean age of 52 years at the time of enterectomy were analyzed, 47% of them males and 53% females. The main etiology of SBS was mesenteric ischemia (73%). Of these patients, 67% had some risk factor associated with atherosclerosis. No significant differences in eating habits were detected between the period before and after surgery. After surgery, 39% of the patients developed a significant weight loss and 79% developed some type of complication, surgical in 34%, infectious in 66% and of both types in 21%. Survival was 9.5 years. Conclusion: Extensive resections of the small bowel may be associated with atherosclerosis and represent an important nutritional risk, with a significant weight loss during the first year, which seems to be related to increased morbidity. Adequate nutritional therapy is associated with increased survival