977 resultados para pre-concentration


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Pós-graduação em Geociências e Meio Ambiente - IGCE

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A new voltammetric method for the determination of Delta(9)-tetrahydrocannabinol (Delta(9)-THC) is described. The voltammetric experiments were accomplished in N-N dimethylformamide/water (9: 1, v/v), using tetrabutylammonium tetrafluoroborate (TBATFB) 0.1 mol/L as supporting electrolyte and a glassy carbon disk electrode as the working electrode. The anodic peak current was observed at 0.0 V (vs. Ag/AgCl) after a 30 s pre-concentration step under an applied potential of -1.2 V (vs. Ag/AgCl). A linear dependence of Delta(9)-THC detection was obtained in the concentration range 2.4-11.3 ng/mL, with a linear correlation coefficient of 0.999 and a detection limit of 0.34 ng/mL. The voltammetric method was used to measure the content of Delta(9)-THC in samples (hemp and hashish) confiscated by the police. The elimination of chemical interferences from the samples was promptly achieved through prior purification using the TLC technique, by employing methanol/water (4: 1, v/v) as the mobile phase. The results showed excellent correlation with results attained by HPLC.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Pós-graduação em Química - IQ

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A novel, simple, rapid and eco-friendly method based on dispersive liquid-liquid microextraction using a bromosolvent was developed to determine six estrogenic mycotoxins (zearalenone, zearalanone, alpha-zearalanol, beta-zearalanol, alpha-zearalenol and beta-zearalenol) in water samples by liquid chromatography-electrospray ionization tandem mass spectrometry in the negative mode (LC-ESI-MS/MS). The optimal conditions for this method include the use of 100 mu L bromocyclohexane as an extraction solvent (using a non-dispersion solvent), 10 mL of aqueous sample (adjusted to pH 4), a vortex extraction time of 2 min, centrifugation for 10 min at 3500 rpm and no ionic strength adjustment. The calibration function was linear and was verified by applying the Mandel fitting test with a 95% confidence level. No matrix effect was observed. According to the relative standard deviations (RSDs), the precision was better than 13% for the repeatability and intermediate precision. The average recoveries of the spiked compounds ranged from 81 to 118%. The method limits of detection (LOD) and quantification (LOQ) considering a 125-fold pre-concentration step were 4-20 and 8-40 ng L-1, respectively. Next, the method was applied to the analysis of the environmental aqueous samples, demonstrating the presence of beta-zearalanol and zearalanone in the river water samples. (C) 2015 Elsevier B.V. All rights reserved.

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Abstracts : The development of analytic methods more selective and sensitive is of great importance for a better quality in the determination of chemical species, therefore increasing the reliability of the results. In this way, the optimization of separation/concentration is still necessary. The use of Molecularly Imprinted Polymers - MIPs have demonstrated to be an efficient tool of analysis with a great potential in minimizing limitations of separation/concentration techniques traditionally employed. In general, the MIPs are obtained by polymerization in the presence of a template to be imprinted so that a polymeric skeleton is formed around the future analyte. In the present work, the template used is Estradiol Valerate (EV), compound used in the hormone replacement therapy (HRT) during climacteric. After the polymerization in bulk and in an anaerobic environment using MAA, EGDMA, AIBN, acetonitrile and VE, the obtained MIP was powdered, sifted (<120 μm) and placed in a soxhlet system containing ethanol at 60 °C, in order to remove the imprinted molecule through six successive washes in periods of 24 hours. The water used in the washings was analyzed using HPLC and spectrophotometry UV/Vis. Then, the obtained MIP was dried at room temperature and 150 mg was inset in SPE cartridges in order to evaluate the polymer's efficiency in the analyte pre-concentration and extraction. To do so, 100,0 mL of VE standard solution (2mg L-1) were pre-concentrated at 4,0 mL min-1 and eluted with 10,0 mL ethanol at 1,0 mL min-1, obtaining recoveries of 53%. Additionally, a NIP (non-imprinting polymer) was prepared to compare the obtained results, in which the recovery was 80%. In the same way, studies were conducted using commercial Strata™-X cartridges, obtaining 53% recovery. Since, the results did not reflect that than was expected, in relation with the MIP efficiency in the recovery, a computational ...