955 resultados para analytical methods


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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Brazilian red wines are very appreciated by consumers from tropical regions, because they typically have aromatic and fruity taste. Thus, the aim of this article is to verify the quality of red wines from wineries located in Northwest region of São Paulo, based on the relationship between physicochemical properties and sensory attributes. Three red wines from this region was evaluated by sensory and analytical methods and it was possible to observe significant differences in the fixed acidity, alcoholic content, total phenolic content and total dry extract. Multidimensional Scaling showed relationship between total phenolic content and astringency, total dry extract and body and the relationship of volatile acidity in the assessment of odor samples. It was possible to see the physicochemical influence in sensory evaluation, indicating the importance of the chemical profile in the elucidation of possible sensory alterations in red wines.

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Indiscriminate and inappropriate use of pesticides in agriculture has been pointed out for increasing health problems and environmental damage. Considering that water resources are the principal destiny of those compounds after application, the present study presents optimization and validation of two simple and effi cient analytical methods for pesticides quantifi cation in both surface and groundwater. Were selected the pesticides more commonly used at Dourados (MS - Brazil), region with intense agricultural activity. Pesticides were preconcentrated by solid-phase extraction using C18 (500 mg) cartridges and then divided in two groups for elution and quantifi cation: 2.4-D and 2.4-DCP were eluted with methanol and quantifi ed by high performance liquid chromatography with ultra-violet detector (HPLC-UV) while atrazine, DIA, DEA, trifl uralin and methyl parathion were eluted with ethylacetate (1:1, v/v) and quantifi ed by gas chromatography with thermionic specifi c detector (GC-TSD). The methods showed satisfactory accuracy (76-107%) and precision (<12%) for the substances analyzed at the fortifi ed levels selected for the study, except for DIA (<51%). Study of pesticide stability also presented good results: C18 cartridges could be stored for at least for 21 days at -20ºC with no signs of the compounds degradability. Both methods limits of quantifi cation of the pesticides (0.22 - 0.48 μg L-1) are in accordance to the levels currently established by the Brazilian national legislation for pesticides in water. Although only the pesticide 2.4-D has been detected in two distinct collection points in the study period of time, this work warns for the requirement of systematical analysis of pesticides presence in water destined to human consume, principally in areas of intense agriculture activity. Such monitoring can provide subsidies for public environmental policies.

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A simple and sensitive method using solid phase microextraction (SPME) and liquid chromatography (LC) with heated online desorption (SPME-LC) was developed and validated to analyze anticonvulsants (AEDs) in human plasma samples. A heated lab-made interface chamber was used in the desorption procedure, which allowed the transference of the whole extracted sample. The SPME conditions were optimized by applying an experimental design. Important factors are discussed such as fiber coating types, pH, extraction time and desorption conditions. The drugs were analyzed by LC, using a C18 column (150 mm 4.6 mm 5 mm); and 50 mmol L1 , pH ¼ 5.50 ammonium acetate buffer : acetonitrile : methanol (55 : 22 : 23 v/v) as the mobile phase with a flow rate of 0.8 mL min1 . The suggested method presented precision (intra-assay and inter-assay), linearity and limit of quantification (LOQ) all adequate for the therapeutic drug monitoring (TDM) of AEDs in plasma.

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This paper reports on the development and validation of a simple and sensitive method that uses solid phase extraction (SPE) and liquid chromatography with ultraviolet detection to analyze fluoxetine (FLX) and norfluoxetine (NFLX) in human plasma samples. A lab-made C18 SPE phase was synthesized by using a sol–gel process employing a low-cost silica precursor. This sorbent was fully characterized by nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM) to check the particles' shape, size and C18 functionalization. The lab-made C18 silica was used in the sample preparation step of human plasma by the SPE-HPLC-UV method. The method was validated in the 15 to 500 ng mL 1 range for both FLX and NFLX using a matrix matched curve. Detection limits of 4.3 and 4.2 ng mL 1 were obtained for FLX and NFLX, respectively. The repeatability and intermediary precision achieved varied from 7.6 to 15.0% and the accuracy ranged from 14.9 to 9.1%. The synthesized C18 sorbent was compared to commercial C18 sorbents. The average recoveries were similar (85–105%), however the lab-made C18 silica showed fewer interfering peaks in the chromatogram. After development and validation, the method using the lab-made C18 SPE was applied to plasma samples of patients under FLX treatment (n ¼ 6). The concentrations of FLX and NFLX found in the samples varied from 46.8–215.5 and 48.0–189.9 ng mL 1 , respectively.

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Throughout the world, biomonitoring has become the standard for assessing exposure of individuals to toxic elements as well as for responding to serious environmental public health problems. However, extensive biomonitoring surveys require rapid and simple analytical methods. Thus, a simple and high-throughput method is proposed for the determination of arsenic (As), cadmium (Cd), copper (Cu), manganese (Mn), nickel (Ni), lead (Pb), and selenium (Se) in blood samples by using inductively coupled plasma–mass spectrometry (ICPMS). Prior to analysis, 200 ml of blood samples was mixed with 500 ml of 10% v/v tetramethylammonium hydroxide (TMAH) solution, incubated for 10 min, and subsequently diluted to 10 ml with a solution containing 0.05% w/v ethylenediamine tetraacetic acid (EDTA) + 0.005% v/v Triton X-100. After that, samples were directly analyzed by ICP-MS (ELAN DRC II). Rhodium was selected as an internal standard with matrix-matching calibration. Method detection limits were 0.08, 0.04, 0.5, 0.09, 0.12, 0.04, and 0.1 mg//L for As, Cd, Cu, Mn, Ni, Pb, and Se, respectively. Validation data are provided based on the analysis of blood samples from the trace elements inter-\comparison program operated by the Institut National de Santé Publique du Quebec, Canada. Additional validation was provided by the analysis of human blood samples by the proposed method and by using electrothermal atomic absorption spectrometry (ETAAS). The method was subsequently applied for the estimation of background metal blood values in the Brazilian population. In general, the mean concentrations of As, Cd, Cu, Mn, Ni, Pb, and Se in blood were 1.1, 0.4, 890, 9.6, 2.1, 65.4, and 89.3 mg/L, respectively, and are in agreement with other global populations. Influences of age, gender, smoking habits, alcohol consumption, and geographical variation on the values were also considered. Smoking habits influenced the levels of Cd in blood. The levels of Cu, Mn, and Pb were significantly correlated with gender, whereas Cu and Pb were significantly correlated with age. There were also interesting differences in Mn and Se levels in the population living in the north of Brazil compared to the south.