The effect of pH on the simultaneous determination of Sulfamethoxazole and Trimethoprim by Ultraviolet Spectrophotometry and Multivariate Calibration

Analytical techniques based on Ultraviolet (UV) spectrophotometry are widely used in pharmaceutical analysis, because they are simple and inexpensive. The choice of pH is critical in the development of univariate methods for pharmaceutical quantitation by UV spectrophotometry since changes may modify the absorption spectrum profile. Similar to univariate methods by UV spectrophotometry changes in pH may influence the predictive ability of multivariate models, affecting the resultant analytical performance. We report herein on the influence of pH on the simultaneous determination of sulfamethoxazole (SMZ) and trimethoprim (TMP) in tablets using UV spectrophotometry and multivariate calibration. Data were recorded using a UV spectrophotometer in the wavelength range of 200 to 350 nm. The experimental matrix was constructed using 36 synthetic samples of SMZ-TMP mixtures. The concentration ranges used for the investigation were 14.0 to 26.0 mg L-1 for SMZ and 2.8 to 5.2 mg L-1 for TMP. The Partial Least Squares (PLS) regression models were generated with full-spectrum and multiple pH levels. At pH 4.3, lower values of relative standard error of prediction (RSEP %) for SMZ (1.83) and TMP (1.13) were obtained. The PLS model at pH 4.3 was used for the quantification of real samples (tablets obtained from 13 different manufacturers) and the results were compared with conventional procedures using high performance liquid chromatography (HPLC).

Green method by diffuse reflectance infrared spectroscopy and spectral region selection for the quantification of sulphamethoxazole and trimethoprim in pharmaceutical formulations

An alternative method for the quantification of sulphametoxazole (SMZ) and trimethoprim (TMP) using diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS) and partial least square regression (PLS) was developed. Interval Partial Least Square (iPLS) and Synergy Partial Least Square (siPLS) were applied to select a spectral range that provided the lowest prediction error in comparison to the full-spectrum model. Fifteen commercial tablet formulations and forty-nine synthetic samples were used. The ranges of concentration considered were 400 to 900 mg g-1SMZ and 80 to 240 mg g-1 TMP. Spectral data were recorded between 600 and 4000 cm-1 with a 4 cm-1 resolution by Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS). The proposed procedure was compared to high performance liquid chromatography (HPLC). The results obtained from the root mean square error of prediction (RMSEP), during the validation of the models for samples of sulphamethoxazole (SMZ) and trimethoprim (TMP) using siPLS, demonstrate that this approach is a valid technique for use in quantitative analysis of pharmaceutical formulations. The selected interval algorithm allowed building regression models with minor errors when compared to the full spectrum PLS model. A RMSEP of 13.03 mg g-1for SMZ and 4.88 mg g-1 for TMP was obtained after the selection the best spectral regions by siPLS

Metabolismo e distribuição do flúor em ovinos jovens tratados cronicamente com fluoreto de sódio

Este estudo teve por objetivo avaliar o metabolismo do flúor (F) em ovinos. Para tanto, utilizaram-se 12 animais, com cinco meses de idade, os quais receberam como dieta base 3% do peso vivo de feno de alfafa e água ad libitum. Os animais foram divididos e constituíram um grupo Controle, que recebeu apenas sal iodado (5g de NaCl/animal + 0,2mg I/kg matéria seca) e, um grupo Tratado, que recebeu sal iodado adicionado de fluoreto de sódio (4,7mg F/kg de peso corporal). Esses sais foram administrados via sonda oro-esofágica, diariamente por um período de 150 dias. Para análise de F, coletaram-se amostras de sangue, urina e fezes e, ao fim do período experimental, após a eutanásia dos animais, coletou-se a glândula pineal e amostras de osso. Também nesta ocasião, coletou-se uma amostra de rim para exame histopatológico. Analisando-se os teores séricos, urinários e ósseos de F, verificou-se que foram significativamente superiores nos animais Tratados em relação aos Controles. Quanto ao F contido na glândula pineal, não houve diferença significativa entre os grupos. Na análise histológica do rim, não foram observadas alterações. Conclui-se que a administração crônica de flúor induz ao acúmulo desse elemento nos ossos, mesmo havendo um alto teor de cálcio na alimentação e esse acúmulo parece não ser nocivo aos animais. Em ovinos, a capacidade orgânica de acúmulo ósseo e excreção urinária do flúor é diferente de outras espécies animais

Environmental quality evaluation of the Vacacaí River, Rio Grande do Sul, Brazil

The water quality of the Vacacaí River was assessed at different sites in the period between winter 2005 and autumn 2006. All samples were analyzed for 52 elements (Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Th, Li, Be, Mg, Al, Ca, V, Cr, Mn, Fe, Ni, Co, Cu, Zn, Ga, As, Se, Rb, Sr, Ag, Cd, In, Cs, Ba, Tl, Pb, Bi, U, Na, K, Hg, B, Mo, Sn, Te, Ti), temperature, pH, ammonia, and alkalinity levels. Water from the Vacacaí River ranged from slightly acidic to alkaline. No difference was observed in the chemical composition at different sites of the Vacacaí River. Levels of Ba, Ca, Sr and Mg increase in the dry seasons and reach their highest concentrations in autumn; Be and U decrease in the dry season and reach their highest concentration in spring. Al, Fe, Cr, Ni, Th, U Mn, Ca and Mg are highly positively related, indicating a common origin. Se and Cu are probably from anthropogenic source, from the rice crops of the margins of the river. Waterborne Al and Fe levels were above the desirable level for drinking water at all sites during all seasons. These results demonstrate the need for constant monitoring of water parameters, which is crucial to ensure water quality for the population of this region. © 2013 Springer-Verlag Berlin Heidelberg

Bioaccumulation and oxidative stress parameters in silver catfish (Rhamdia quelen) exposed to different thorium concentrations

The objective of this study was to evaluate the effect of chronic thorium (Th) exposure on bioaccumulation, metabolism (through biochemical parameters of the muscle) and oxidative parameters (lipidic peroxidation levels and antioxidant enzymes in the gills and in the hepatic and muscular tissues) of silver catfish (Rhamdia quelen). Silver catfish juveniles were exposed to different waterborne Th levels (in lg L1 ): 0 (control), 25.3 ± 3.2, 80.6 ± 12.0, 242.4 ± 35.6, and 747.2 ± 59.1 for 30 d. The gills and skin were the organs that accumulated the highest Th levels. The increase in the waterborne Th concentration corresponded to a progressive increase in the Th levels in the gills and kidney. Chronic Th exposure causes alterations in the oxidative parameters of silver catfish gills, which are correlated with the Th accumulation in this organ. The levels of GST decreased in the gills of fish exposed to 747.2 lg L1 Th and SOD activity decreased in silver catfish exposed to 242.4 and 747.2 lg L1 Th. In addition, the increase in the LPO in the gills exposed to 242.4 and 747.2 lg L1 Th suggests that higher oxidative damage occurred in the gills. However, in the liver and muscle, these alterations occurred mainly in the lowest waterborne Th level. Metabolic intermediates in the muscle were altered by Th exposure, but no clear relationship was found.Fil: Kochhann, Daiani. Universidade Federal de Santa Maria.; BrasilFil: Pavanato, Maria A.. Universidade Federal de Santa Maria.; BrasilFil: Llesuy, Susana Francisca. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Química Analítica y Fisicoquímica; ArgentinaFil: Correa, Lizelia M.. Universidade Federal de Santa Maria.; BrasilFil: Konzen Riffel, Ana P.. Universidade Federal de Santa Maria.; BrasilFil: Loro, Vania L.. Universidade Federal de Santa Maria.; BrasilFil: Mesko, Márcia F.. Universidade Estadual do Rio Grande do Sul ; Brasil. Universidade Federal de Santa Maria.; BrasilFil: Flores, Érico M.M.. Universidade Federal de Santa Maria.; BrasilFil: Dressler, Valderi L.. Universidade Federal de Santa Maria.; BrasilFil: Baldisserotto, Bernardo. Universidade Federal de Santa Maria.; Brasi