Um método analítico baseado na extração em fase sólida e cromatografia líquida acoplada à espectrometria de massas tandem (LC-ESI-MS-MS) foi desenvolvido e validado para a determinação e confirmação de dezoito agrotóxicos (herbicidas, inseticidas e fungicidas) e dois metabólitos em amostras de água. Os limites de detecção variaram de 0,4 a 40,0 ng L -1 e os limites de quantificação de 4,0 a 100,0 ng L -1 . Foi obtida boa linearidade, com r 2 > 0,99 para todos os compostos. As recuperações, para 95% dos compostos, variaram de 70 a 120%, com RSDs menores que 21% para todos. Através do monitoramento de reações múltiplas (MRM), foram selecionadas duas diferentes transições íon precursor-íon produto para cada agrotóxico. A metodologia proposta pode ser usada para a determinação de resíduos de agrotóxicos em águas de superfície e potável, em concordância com a Lei n° 518 do Ministério da Saúde, Brasil, e com os parâmetros da União Européia para água potável (Directive 98/83/EC).An analytical method using solid-phase extraction and liquid chromatography coupled to electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS) was developed and validated for the determination and confirmation of eighteen polar pesticides (herbicides, insecticides and fungicides) and two metabolites in water samples. The limits of detection varied between 0.4-40.0 ng L -1 and the limits of quantification between 4.0-100.0 ng L -1 . Good linearity with r 2 > 0.99 for all compounds was obtained. The recovery for 91% of the accuracy experiments varied from 70 to 120%, with RSD below 21% for all. Through multiple reaction monitoring (MRM) two different precursor ion-product ion transitions were selected for each pesticide. The proposed methodology can be used for the convenient and effective determination of pesticide residues in surface and drinking waters in accordance with Law No. 518 of the Ministry of Health, Brazil, and the European Union Directive on drinking water quality (98/83/EC).
Zinc demonstrates protective and antioxidant properties at physiological levels, although these characteristics are not attributed at moderate or high concentrations. Zinc toxicity has been related to a number of factors, including interference with antioxidant defenses. In particular, the inhibition of glutathione reductase (GR) has been suggested as a possible mechanism for acute zinc toxicity in bivalves. The present work investigates the biochemical effects of a non-lethal zinc concentration on antioxidant-related parameters in gills of brown mussels Perna perna exposed for 21 days to 2.6 μM zinc chloride. After 2 days of exposure, zinc caused impairment of the antioxidant system, decreasing GR activity and glutathione levels. An increase in antioxidant defenses became evident at 7 and 21 days of exposure, as an increase in superoxide dismutase and glutathione peroxidase activity along with restoration of glutathione levels and GR activity. After 7 and 21 days, an increase in cellular peroxides and lipid peroxidation end products were also detected, which are indicative of oxidative damage. Changes in GR activity contrasts with protein immunoblotting data, suggesting that zinc produces a long lasting inhibition of GR. Contrary to the general trend in antioxidants, levels of peroxiredoxin 6 decreased after 21 days of exposure. The data presented here support the hypothesis that zinc can impair thiol homeostasis, causes an increase in lipid peroxidation and inhibits GR, imposing a pro-oxidant status, which seems to trigger homeostatic mechanisms leading to a subsequent increase on antioxidant-related defenses.
A simple and sensitive method to determine parts per billion (ppb) of atmospheric formaldehyde in situ, using chromotropic acid, is described. A colorimetric sensor, coupled to a droplet of 15.5 microL chromotropic acid, was constructed and used to sample and quantify formaldehyde. The sensor was set up with two optical fibers, a light emitting diode (LED) and two photodiodes. The reference and transmitted light were measured by a photodetection arrangement that converts the signals into units of absorbance. Air was sampled around the chromotropic acid droplet. A purple product was formed and measured after the sampling terminated (typically 7 min). The response is proportional to the sampling period, analyte concentration and sample flow rate. The detection limit is approximately 2 ppb and can be improved by using longer sampling times and/or a sampling flow rate higher than that used in this work, 200 mL min-1. The present technique affords a simple, inexpensive near real-time measurement with very little reagent consumption. The method is selective and highly sensitive. This sensor could be used either for outdoor or indoor atmospheres.
Nitrogen dioxide is an important atmospheric contaminant, classified as a criteria pollutant in the United States. It can be sensitively determined by the simple colorimetric Griess-Saltzmann method. This can constitute the basis of an inexpensive sensitive instrument based on gas-permeable liquid core waveguide tubes that allow long path absorbance measurement. Nitrous (HONO) acid is often present in the atmosphere along with NO 2 . Nitrous acid concentration can be significant relative to NO 2 , especially at night-time when photodecomposition of HONO is no longer operative. Griess-Saltzman chemistry cannot differentiate between HONO and NO 2 . In the present paper, we have explored the possibility of simultaneously determining both analytes by using more than one collector with dimensional differences. Presented results show that differences in either length or wall thickness can permit such differentiation.
The design and characteristics of a novel electrochemical system, which uses a drop as a renewable electroanalytical sensor, are described. This article describes the performance of the electrochemical system, the coupling of the experimental arrangement with flow injection technique and a demonstration of its applicability for the measurement of sulfide. The method is based on renewable drops of ferricyanide ions, buffered by borate. The ferrocyanide ions, product of the reaction between ferricyanide and sulfide ions, are oxidized on a platinum microelectrode and the current measured is related to sulfide concentration. The measurements can be done in continuous or static flow mode. In continuous mode, the detection limit is 5.0 Â 10 À5 mol L À1 .
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