993 resultados para Mass spectrometer
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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ABSTRACT: Analytical procedures for U-Pb isotope dilution analyses at the Pará-Iso isotope geology laboratory of the Federal University of Pará (UFPA) are described in detail. The procedures are applied to zircon, titanite, rutile, apatite, columbite-tantalite and whole rock. Reagent preparation and chemical processing are done in clean-room conditions. Samples are dissolved using Teflon™ microcapsules in steel jacket Teflon™ Parr Instrument™ bomb or Teflon™ screw cap containers. U and Pb are separated using anion exchange AG 1x8 resin columns. Typical blanks for mineral sample amounts of 0.01 to 1.0 mg are less than 1 pg U and 20-30 pg Pb. Isotope analysis of the U and Pb from the same filament are carried out using a Finnigan MAT 262 mass-spectrometer in static and dynamic modes. The current analytical level is demonstrated on analyses of international standard zircon 91500 with three different 235U-205Pb and 235U-208Pb isotope tracers and whole rock standards. Results of analyses of two zircon samples are also presented.
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Pós-graduação em Zootecnia - FMVZ
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Pós-graduação em Zootecnia - FMVZ
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Pós-graduação em Engenharia e Ciência de Alimentos - IBILCE
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Pós-graduação em Agronomia (Agricultura) - FCA
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Herbs and spices have long been used to improve the flavour of food without being considered as nutritionally significant ingredients. However, the bioactive phenolic content of these plant-based products is currently attracting interest.In the present work, liquid chromatography coupled to high-resolution/accurate mass measurement LTQ-Orbitrap mass spectrometry was applied for the comprehensive identification of phenolic constituents of six of the most widely used culinary herbs (rosemary, thyme, oregano and bay) and spices (cinnamon and cumin). In this way, up to 52 compounds were identified in these culinary ingredients, some of them, as far as we know, for the first time. In order to establish the phenolic profiles of the different herbs and spices, accurate quantification of the major phenolics was performed by multiple reaction monitoring in a triple quadrupole mass spectrometer. Multivariate statistical treatment of the results allowed the assessment of distinctive features among the studied herbs and spices. (C) 2014 Elsevier Ltd. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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An analytical method based on liquid chromatography with positive ion electrospray ionization (ESI) coupled to tandem mass spectrometry detection was developed for the determination of pantoprazole (CAS 102625-70-7) in human plasma using lansoprazole (CAS 103577-45-3) as the internal standard. The analyte and internal standard were extracted from the plasma samples by liquid/liquid extraction using diethyl-ether/dichloromethane (70:30; v/v) and chromatographed on a C-8 analytical column. The mobile phase consisted of acetonitrile/water/methanol (57:25:18; v/v/v) + 10 mmol/l acetic acid + 20 mmol/l ammonium acetate. The method has a chromatographic total run time of 4.5 min and was linear within the range 5.0-5,000 ng/mL. Detection was performed on a triple quadrupole tandem mass spectrometer by Multiple Reaction Monitoring (MRM). The intra- and inter-run precisions calculated from quality control (QC) samples were 4.2% and 3.2%, respectively. The accuracies as determined from QC samples were -5.0% (intra-run) and 2.0% (inter-run). The method herein described was employed in a bioequivalence study of two tablet formulations of pantoprazole.
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Currently the study of important molecular compounds present in low abundance in some tissues has been a challenge for proteomic analysis classic. An analysis requires more exploratory investigation of small regions of a tissue or a group of cells. MALDI Imaging Technology (MSI) is an application of mass spectrometry facing the chemical analysis of intact tissues. Thus, advances in mass spectrometry MALDI being obtained by the integration of histology, the best methods and automation are the main tools of data analysis. This tool has become essential to analyze the spatial distribution of peptides and proteins throughout the tissue sections, providing an enormous amount of data with minimum sample preparation. Thus, the aim of this study was to develop the technique of MALDI Imaging using tissue from glioblastoma multiforme (GBM), a form of most common malignant tumor in the brain. For this we used the printer chemical ChIP-1000 (Chemical Inkjet Printer, Shimadzu) and mass spectrometer type Maldi-ToF-ToF (Axima Performance, Shimadzu), a search of the identifications were performed in databases such as SwissProt. We identified more than forty proteins with diverse functions such as proteins F-actin-capping and Thymosin to the structure and organization cellular and proteins such several Tumor necrosis factor receptor development-related pathology. The development of this technique will permit to carry-out proteomic analysis directly into the tissue, enabling earlier diagnosis of diseases, as well as the identification and characterization of potential biomarkers of disease.
Desenvolvimento de uma plataforma analítica para aquisição de imagens moleculares em tecidos animais
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Objectives: the aim of this work was to define the range of possible values for each isotope of carbon-13 and nitrogen-15 for cocaine and marijuana seized in Botucatu-SP, with the intention of distinguishing the geographical origin of the drug. Materials and Methods: samples of marijuana and cocaine were collected at the time of incineration. Then, at the Stable Isotope Center from São Paulo State University in Botucatu, São Paulo, Brazil, samples of marijuana were subjected to the drying process and subsequent grinding. Samples of cocaine were not submitted to the processes of drying and grinding because they were already in adequate granulometry. Subsequently, the samples of both drugs were weighed in accordance with the standards for carbon-13 and nitrogen-15. Lastly, CO2 and N2 gases were obtained from the samples through the elemental analyzer. They were then analyzed in a mass spectrometer to obtain values of δ13C and δ15N in ‰. Results and Discussion: the results of marijuana allowed for comparison with regions of Queensland, Australia, according to the range of δ13C between -29.9 ‰ and -29.3 ‰ and δ15N range from 4.1 ‰ to 5.8 ‰. The results were also consistent with those of the state of Pará, Brazil, where the values of δ13C and δ15N were -30.3 ± 0.7 ‰ and 5.0 ± 1.3 ‰, respectively. Also the results were in accordance with those from the state of Mato Grosso do Sul, Brazil, in which δ13C values varied by -28.7 ± 1.3 ‰, and δ15N values varied by 6.6 ± 1.1 ‰, respectively. In both regions, the samples identified as being from Pará and Mato Grosso do Sul showed an overlap. In addition, the results fitted with data from the state of Maranhão, in which the values of δ13C and δ15 N were -28.8 ± 1.6 ‰ and 2.9 ± 2.5 ‰, respectively. In the case of cocaine, the present study could not be related to the results from the literature. One possible explanation may be related to the non-purification of ...
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A study was conducted to determine the optimal time for collecting the breath examination urea breath marked with the stable isotope 13C. We selected patients before undergoing the examination of endoscopy at the Endoscopy Section of the University Hospital of Botucatu - SP. A screening was performed to determine which patients wanted and could participate. Before performing endoscopy basal sample was collected from the patient and then the labeled urea ingested. The blows were collected in double every 2.5 minutes until an interval of 30.0 minutes after were collected every 5.0 minutes until the time of 45.0 minutes . The samples were analyzed in a mass spectrometer for isotope ratio, located in the center of Stable Isotopes, Institute of Biosciences, UNESP - Botucatu campus. The data were studied and arranged in the form of graphics to better interpretation of results. Based on the obtained results it was determined that a standby time of 15.0 minutes to collect the wind is sufficient for accurate diagnosis and effective