Otimização evalidação de métodos analíticos para a determinação simultânea de tuberculostáticos (4-FDC) por CLAE/DAD e CLUE/ DAD

Tuberculosis is a serious disease, but curable in practically 100% of new cases, since complied the principles of modern chemotherapy. Isoniazid (ISN), Rifampicin (RIF), Pyrazinamide (PYR) and Chloride Ethambutol (ETA) are considered first line drugs in the treatment of tuberculosis, by combining the highest level of efficiency with acceptable degree of toxicity. Concerning USP 33 - NF28 (2010) the chromatography analysis to 3 of 4 drugs (ISN, PYR and RIF) last in average 15 minutes and 10 minutes more to obtain the 4th drug (ETA) using a column and mobile phase mixture different, becoming its industrial application unfavorable. Thus, many studies have being carried out to minimize this problem. An alternative would use the UFLC, which is based with the same principles of HPLC, however it uses stationary phases with particles smaller than 2 μm. Therefore, this study goals to develop and validate new analytical methods to determine simultaneously the drugs by HPLC/DAD and UFLC/DAD. For this, a analytical screening was carried out, which verified that is necessary a gradient of mobile phase system A (acetate buffer:methanol 94:6 v/v) and B (acetate buffer:acetonitrile 55:45 v/v). Furthermore, to the development and optimization of the method in HPLC and UFLC, with achievement of the values of system suitability into the criteria limits required for both techniques, the validations have began. Standard solutions and tablets test solutions were prepared and injected into HPLC and UFLC, containing 0.008 mg/mL ISN, 0.043 mg/mL PYR, 0.030 mg.mL-1 ETA and 0.016 mg/mL RIF. The validation of analytical methods for HPLC and UFLC was carried out with the determination of specificity/selectivity, analytical curve, linearity, precision, limits of detection and quantification, accuracy and robustness. The methods were adequate for determination of 4 drugs separately without interfered with the others. Precise, due to the fact of the methods demonstrated since with the days variation, besides the repeatability, the values were into the level required by the regular agency. Linear (R> 0,99), once the methods were capable to demonstrate results directly proportional to the concentration of the analyte sample, within of specified range. Accurate, once the methods were capable to present values of variation coefficient and recovery percentage into the required limits (98 to 102%). The methods showed LOD and LOQ very low showing the high sensitivity of the methods for the four drugs. The robustness of the methods were evaluate, facing the temperature and flow changes, where they showed robustness just with the preview conditions established of temperature and flow, abrupt changes may influence with the results of methods

Diferenciais de rendimentos por gênero: uma análise dos efeitos composição e estrutura salarial no Brasil (1976, 1987, 1996 e 2009)

This study aims to analyze the income differentials by gender in Brazil, in the years 1976, 1987, 1996 and 2009. Specifically, there are two objectives. First, attempt to analyze the importance of the effects of composition and wage structure in the job market. In the second, to verify which socioeconomic variables explain the effects of composition and wage structure in the job market. The information in this study was obtained from the microdata of Pesquisa Nacional por Amostra de Domicílios (PNAD) regarding the respective years. In the first stage of the methodology we used: the index of income distribution Theil-T; the income gap decompositions proposed by Oaxaca (1973) and Blinder (1973); and Firpo et al. (2007). In the second stage we applied the RIF regression method (Recentered Influence Function) of Firpo et al. (2007). The results show that income inequality is higher among men than among women in the country. It was observed that the component of inequality between people of the same gender represented the largest share in the decomposition of income inequality between genders. It was found, in the decomposition of the average income, a downward trend of income gap, but the differential remains favorable to the men. We noticed that the impact of the composition effect in reducing the gap was offset by the positive effect of wage structure. Regarding the distribution quantis, income differential between genres appeared greater at the bottom, in the years 1976, 1987 and 2009; and at the top of the distribution, in 1996 featuring, respectively, the sticky floor and glass ceiling effects in Brazil. As for the decomposition of the RIF, it turns out that the composition effect assisted in the downfall of the income gap between 1976 and 2009, but was offset by the positive effect of the wage structure in quantis 10th, 50th, and 90th. The main socioeconomic variables influenced the drop in income gap were: the composition effect, the manual labor occupations, service sector and low-grade and high school, and the wage structure effect, schooling low and high experience professional and technical occupations and urban centers

Aplicação das técnicas eletroanalíticas (voltametria cíclica e de pulso diferencial) usando o eletrodo de diamante dopado com boro para o estudo da isoniazida, etambutol, rifampicina e pirazinamida

In this work a study was done using electrochemical cyclic voltammetry and differential pulse voltammetry for isoniazida (INH), ethambutol (EMB), rifampicina (RIF) and pyrazinamide (PZA) using the electrode boron-doped diamond (BDD) as working electrode. It also verified the applicability of the technique of differential pulse voltammetry in the quantification of the active compounds used in the treatment of tuberculosis, subsequently applying in samples of pharmaceutical formulation. Among the four active compounds studied, isoniazid showed the best results for the detection and quantification using differential pulse voltammetry. At pH 4 and pH 8, for the calibration curves to INH showed good linearity, with quantification limits of 6.15 mmol L-1 (0,844 ppm) and 4.08 mmol L-1 (0.560 ppm) for the respective pH. The proposed method can be used to determine drug isoniazid, for recovery values were obtained in approximately 100%