942 resultados para SPME sampling
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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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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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The present study aimed to evaluate the volatiles profile of red mombin (Spondias purpurea) pulp and its powder produced by spray-drying (SD) as an example to show utility of headspace solid-phase microextraction (HS-SPME) in the analysis of parameters such as the quality and stability of fruit products. Volatiles profiles of the pulp were identified by gas chromatography-mass spectrometry (GC-MS), quantified by gas chromatography-flame ionization detector (GC-FID) and compared to the profile of the powder stored at 0, 60 and 120 days in plastic (PP) or laminated packages (LP). The results showed that the technique was able to identify 36 compounds in the red mombin pulp, 17 out of which have been described for the first time in this fruit, showing that red mombin fresh pulp appears to be unique in terms of volatiles composition. However, only 24 compounds were detected in the powder. This decrease is highly correlated (r(2) = 0.99), at least for the majority of compounds, to the degree of volatility of compounds. Furthermore, the powder stored in PP or LP showed no statistical differences in the amounts of its components for a period of 120 days of storage. Finally, this work shows how HS-SPME analysis can be a valuable tool to assess the quality and stability of fruit products.
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In the seed production system, genetic purity is one of the fundamental requirements for its commercialization. The present work had the goal of determined the sample size for genetic purity evaluation, in order to protect the seed consumer and the producer and to evaluate the sensitivity of microsatellite technique for discriminating hybrids from their respective relatives and for detecting mixtures when they are present in small amounts in the samples. For the sequential sampling, hybrid seeds were marked and mixed in with the seed lots, simulating the following levels of contamination: 0.25, 0.5, 1.0, 2.0, 4.0, and 6.0%. After this, groups of 40 seeds were taken in sequence, up to a maximum of 400 seeds, with the objective of determining the quantity of seeds necessary to detect the percentage of mixture mentioned above. The sensitivity of microsatellite technique was evaluated by mixing different proportions of DNA from the hybrids with their respective seed lines. For the level of mixture was higher than 1:8 (1P1:8P2; 8P1:1P2), the sensitivity of the marker in detecting different proportions of the mixture varied according to the primer used. In terms of the sequential sampling, it was verified that in order to detect mixture levels higher than 1% within the seed lot- with a risk level for both the producer and the consumer of 0.05- the size of the necessary sample was smaller than the size needed for the fixed sample size. This also made it possible to reduce costs, making it possible to use microsatellites to certify the genetic purity of corn seeds lots.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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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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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Direct immersion SPME-GC-MS-MS was used for the analysis of steroids in water at part-per-trillion(ppt) and lower concentrations. The method was validated and extended to real sample analysis. The method were linear from 0.01 to 5 ng/ml with precision less than 10% relative standard deviation for a steroid mixture at 1 ng/ml. Limit of quantitation and limit of detection was found to be 200- 1200 pg/L and 30-200 pg/L respectively and recoveries ranged from 88-103 %. To understand the extraction efficiency of the fiber, a depletion study was performed. The fiber/ sample partition coefficients for the steroids were determined to be 1.0 x 104 to 1.5 x 104 . The extraction was performed without derivatization or the use of an internal standard. SPMEGC-MS-MS effectively demonstrated ultra-trace level detection of steroids in water.
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Pós-graduação em Química - IQ
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The steady-state average run length is used to measure the performance of the recently proposed synthetic double sampling (X) over bar chart (synthetic DS chart). The overall performance of the DS X chart in signaling process mean shifts of different magnitudes does not improve when it is integrated with the conforming run length chart, except when the integrated charts are designed to offer very high protection against false alarms, and the use of large samples is prohibitive. The synthetic chart signals when a second point falls beyond the control limits, no matter whether one of them falls above the centerline and the other falls below it; with the side-sensitive feature, the synthetic chart does not signal when they fall on opposite sides of the centerline. We also investigated the steady-state average run length of the side-sensitive synthetic DS X chart. With the side-sensitive feature, the overall performance of the synthetic DS X chart improves, but not enough to outperform the non-synthetic DS X chart. Copyright (C) 2014 John Wiley &Sons, Ltd.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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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)