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  • Author or Editor: C.M.M. Silveira x
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This study aimed to optimize and validate methods for the analysis of thiamin and folic acid in fortified rice, pure and mixed to the milled rice (raw and cooked). The analysis was performed by high-performance liquid chromatography coupled to a diode array detector (HPLC—DAD). Different mobile phases were tested. Different ratios of organic modifier, pH ranges, triethylamine concentrations, and flow rates were used. For the validation, tests of recovery, repeatability, linearity, limit of detection (LOD), and limit of quantification (LOQ) were performed. The optimized methods showed good resolution of vitamins’ peaks, excellent recovery (82.6 to 104%), repeatability with relative standard deviation of peak areas, and retention times less than 10% and high coefficients of determination (0.9998 for thiamin and 0.9997 for folic acid). The LOD and LOQ were 0.00193 μg and 0.0193 μg for thiamin and 0.000934 μg and 0.00934 μg for folic acid. The optimized methods demonstrated reliability and sensitivity in the detection and quantification of these vitamins in fortified rice, pure and mixed to milled rice (raw and cooked). Furthermore, the methods were performed in isocratic mode, with short run time (<13 min), reflecting positively on the economy of reagents and analysis times.

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Authors: R. Parise Filho, A. Araújo, M. Santos Filho, J. Matos, M. Silveira and C. Brandt

Abstract  

Oxamniquine (OXA) is a schistosomicide agent that causes some adverse effects in central nervous system. Intending to improve OXA therapeutic properties, a polymeric prodrug was designed. Currently, there is an increasing interest of thermal analytical techniques in the pharmaceutical area, so differential thermal analysis (DTA) and thermogravimetry (TG) were carried out to evaluate the thermal behavior of OXA, polymethacrylic acid (PMA), [poly(methacrylic-co-oxamniquine methacrylate)acid] (PMOXA) and physical mixture (OXA+PMA). The thermoanalytical profile of the physical mixture showed characteristic events of the thermal decomposition of OXA and PMA. Distinctly, PMOXA DTA curve did not show an endothermic peak at 148.5C indicating that the drug was incorporated into the polymeric system. These results were corroborated by the IR spectroscopy and X-ray diffraction data.

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Authors: J. A. S. Júnior, J. J. R. F. Cardoso, C. M. Silva, S. V. Silveira and R. S. Amaral

Summary  

Seventy nine samples, including soil and rock, were collected from the agrestic region of the State of Pernambuco, Brazil. The activity concentrations of 238U and 226Ra in the samples were determined by gamma-spectrometry using an HPGe detector. The concentrations of 238U were 22 Bq . kg-1 to 22 kBq . kg-1. The concentrations of 226Ra were 14 Bq . kg-1   to 17 kBq . kg-1. The 238U/226Ra ratios in the soil were 0.7 to 3.4 (arithmetic mean 1.7). The radiometric data were evaluated to explain 238U and 226Ra migration in the soil and the possible consequences to the environment.

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Authors: S.M. Silveira, A. Cunha Jr., M. Maraschin, S. Verruck, F.L. Secchi, G. Scheuermann, E.S. Prudencio, N. Fronza and C.R.W. Vieira

The antioxidant and antimicrobial activities of extracts of 12 plant species growing in Brazil were determined. Antimicrobial activity against 12 food-related bacterial species was studied using the disc-diffusion, MIC, and MBC methods. Campomanesia eugenioides extract was the most active against the tested Gram-positive bacteria, whereas Parapiptadenia rigida bark extract presented the highest activity against the evaluated Gram-negative bacteria (MIC and MBC of 0.075 and 0.62 mg ml−1, respectively, against Pseudomonas aeruginosa). Those two extracts also presented high phenolic content and high DPPH and ABTS radical scavenging ability. C. eugenioides extract presented high Fe2+ chelating capacity. The results of the present study demonstrate that, among the evaluated extracts, P. rigida bark and C. eugenioides, both Brazilian native species, presented the highest potential of application as natural antimicrobial and antioxidant agents.

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Summary

A stability-indicating liquid chromatographic (LC) method with UV detection was developed for the determination of doripenem in the marketed formulation (Doribax® 500 mg, powder for injection). A forced degradation study was conducted according to available guidelines and main references. Thermal, oxidizing, acidic and basic stress conditions were assayed to show the stability-indicating power of the method. Chromatographic separation was achieved using an isocratic elution method in a reversed-phase system using a mobile phase prepared from phosphate buffer and acetonitrile. Extensive degradation was observed under thermal, oxidative and basic treatment, and the products formed were detected without interference in the analysis of doripenem. To verify the efficiency of chromatographic run, the system suitability was studied. The theoretical plates (N = 5498.3) and tailing factor (tf = 0.951) were constant during repeated injections. The retention time of doripenem was 7.35 min and the method was validated within the concentration range 5–50 μg mL−1 (r = 0.999). Adequate results were obtained that indicate repeatability (RSD % = 1.03–1.37), inter-day precision (RSD % = 0.51) and accuracy. In comparison to spectrophotometric and microbiological methods, statistical analysis showed no significant difference between the obtained results. The proposed method was successfully applied to doripenem quantification, showing it is applicable to determine the antibiotic in the presence of degradation products and also that is a reliable method for routine analysis.

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Authors: C. M. Silva, R. S. Amaral, A. Amaral, J. A. Santos Júnior, D. C. Santos, L. E. Lima and S. V. Silveira

Summary  

Studies performed by the Brazilian Nuclear Corporation (NUCLEBRAS), in collaboration with the Geological Survey Company of Brazil (CPRM), identified high levels of natural uranium in the districts of Pedra and Venturosa, in the rural region of the state of Pernambuco (PE) - Brazil, where the maximum value found in rocks was 22,000 mg.

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