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Cromatografia líquida multidimensional e espectrometria de massas em tandem para análise direta de fármacos em fluidos biológicos: da escala convencional à miniaturizada; Multidimensional liquid chromatography and tandem mass spectrometry for the direct analysis of grugs in biofluids: from the conventional to the miniaturized scale

Santos Neto, Álvaro José dos
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 31/08/2007 PT
Relevância na Pesquisa
45.69%
A análise de fármacos e outras moléculas relacionadas em fluidos biológicos é essencial no âmbito farmacêutico. Atualmente, a demanda por análises rápidas e mais complexas impulsiona a química analítica para o desenvolvimento de soluções inovadoras. A cromatografia líquida multidimensional com acoplamento de colunas para injeção direta de fluidos biológicos tem ganhado atenção nos últimos anos. Ao mesmo tempo, o acoplamento entre cromatografia líquida e espectrometria de massas proporcionou marcante desenvolvimento científico na área biomédica e bioquímica. Esta tese apresenta os diversos estágios na redução da escala em sistemas de column switching utilizando colunas RAM, para a análise de fármacos em fluidos biológicos. Na escala convencional, com colunas de 4,6 mm de diâmetro interno, desenvolveu-se um sistema para a análise de fluoxetina em plasma. A metodologia desenvolvida foi adequadamente validada para aplicação na monitorização terapêutica, com tempo de análise de 20 minutos (incluído o preparo de amostras) e consumo de apenas 100 µL de amostra. Avaliou-se a escala microbore (2,1 mm), a qual apresentou excelente potencialidade para o acoplamento com a espectrometria de massas utilizando ionização por electrospray. Na primeira etapa em escala capilar...

Estudo de métodos visando à análise direta de alumina, cimento e quartzo em ICP OES; Studies of methods aiming the direct analysis of alumina, cement and quartz by ICP OES

Souza, Alexandre Luiz de
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 29/07/2011 PT
Relevância na Pesquisa
65.76%
O objetivo deste estudo foi avaliar parâmetros para o desenvolvimento de métodos visando à determinação elementar em alumina, cimento e quartzo por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) com amostragem de suspensão. Alguns elementos foram investigados como possíveis candidatos a padrões internos (PIs) Be, Dy, Gd, In, La, Sc, Y, Yb eTl. Amostras de material de referência certificado (CRM) de alumina (Alumina Reduction Grade 699), de cimento Portland (1889a Blended with Limestone e 1886a White Portland cement with low iron) do National Institute of Standard and Technology (NIST), e amostras de quartzo, cedidos pelo Departamento de Física da Universidade Federal de São Carlos (UFSCar), denominados T-4FI, T-2FI e T-4GR, foram utilizadas na otimização instrumental, no desenvolvimento e na avaliação da exatidão do método. Nanopartículas de sílica de alta pureza (Wacker HDK® T40), Wacker Chemie AG foram utilizadas no estudo de adsorção dos elementos e padrões internos como proposta de produção de material calibrante para a análise direta de sólidos. Para a escolha dos PIs foram construídos gráficos de correlação usando valores de potenciais de excitação, energias de ionização e temperaturas de fusão dos analitos e dos candidatos a PIs. Análise exploratória por agrupamentos hierárquicos (HCA) e análise dos componentes principais (PCA)...

Contribuição ao estudo da estabilidade de edifícios de andares múltiplos em aço; Contribution to the study of stability of steel multi-storey buildings

Camargo, Rafael Eclache Moreira de
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 20/08/2012 PT
Relevância na Pesquisa
45.66%
Este trabalho apresenta uma análise comparativa de diferentes sistemas estruturais para um edifício de 20 pavimentos. Cada um dos modelos foi dimensionado através dos princípios do método da análise direta, presente na ABNT NBR 8800:2008. O método da amplificação dos esforços solicitantes (MAES) foi usado para se obter de forma simplificada os esforços atuantes nos elementos do edifício considerando os efeitos locais e globais de segunda ordem. A incidência do vento foi simulada de duas formas diferentes. Na primeira, chamada de uniforme, o vento foi aplicado sem excentricidade, gerando apenas o efeito de tombamento nas estruturas. Na segunda hipótese, considerou-se uma excentricidade devida aos efeitos de vizinhança, prescrita pela ABNT NBR 6123:1988, responsável por ocasionar o tombamento e a torção dos edifícios. Todas as análises numéricas foram repetidas fazendo o uso de outro método simplificado de segunda ordem, conhecido como P-Delta. Por meio dos resultados obtidos, constatou-se que a possibilidade de se reduzir a sobrecarga para o dimensionamento de pilares proporciona uma economia de material, mas, por outro lado, tem como consequência o aumento do tempo de análise, pois exige a utilização de diferentes combinações de cálculo para o dimensionamento de vigas e pilares. A estratégia utilizada para simular os efeitos de vizinhança mostrou-se satisfatória...

Determinação direta de elementos potencialmente tóxicos em arroz por GF AAS: desenvolvimento de métodos e aplicações; Direct determination of potentially toxic elements in rice by GF AAS: methods development and applications

Silvestre, Daniel Menezes
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 26/03/2013 PT
Relevância na Pesquisa
55.76%
O arroz é um dos alimentos mais consumidos no mundo, caracterizando-se como a base da alimentação para mais da metade da população mundial. De acordo com a Organização Mundial da Saúde (WHO), a ingestão de alimentos contaminados é uma das principais vias de absorção de elementos potencialmente tóxicos pelo ser humano. Por esse motivo, órgãos de fiscalização têm estabelecidos limites máximos permitidos desse tipo de elemento nos alimentos. Nesse sentido, o desenvolvimento de métodos e aplicações visando à determinação de elementos com caráter tóxico, tais como o Al, As, Cd e Pb em alimentos é de suma importância. Nesse projeto, foram desenvolvidos métodos para determinações diretas de Al, As, Cd e Pb em arroz por espectrometria de absorção atômica com forno de grafite e amostragem direta de sólidos (SS-GF AAS) que tem se mostrado uma técnica promissora especialmente devido à sua elevada sensibilidade e detectabilidade, além de dispensar morosos processos de decomposição de amostra. A adequada otimização do programa de aquecimento aliado ao uso de modificadores químicos adequados possibilitou o uso de calibração aquosa. Parâmetros importantes como o tamanho de partícula, massa de amostra e segregação de analito foram investigados. Observou-se que partículas inferiores a 100 µm geravam resultados precisos. A massa mínima ideal de amostra de arroz a ser utilizada na análise foi em torno de 300 µg. A massa máxima recomendada foi 500 µg. Segregação de Al e Cd não foram observadas na amostra de arroz. A segunda parte do projeto envolveu a aplicação do método de análise desenvolvido em amostras de arroz comercializadas na cidade de São Paulo. Investigou-se também a influência dos processos de lavagem e cozimento dos grãos sobre a concentração de Al...

Determinação direta de silício em folhas de cana-de-açúcar por espectrometria de emissão óptica com plasma induzido por laser (LIBS); Direct determination of silicon in sugarcane leaves by laser-induced breakdown spectroscopy (LIBS)

Souza, Paulino Florêncio de
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 19/12/2012 PT
Relevância na Pesquisa
45.73%
A cultura da cana-de-açúcar no Brasil é uma das atividades mais relevantes na agroindústria nacional devido ao alto potencial de produção e elevada importância econômica de seus subprodutos como e.g. açúcar e etanol. Embora o Si não seja considerado um elemento essencial, a adubação silicatada tem proporcionado aumentos apreciáveis na produtividade da cana-de-açúcar e na resistência a algumas pragas e doenças. Ainda não existem métodos bem estabelecidos para a determinação de Si em material vegetal visando à diagnose foliar. O objetivo deste trabalho foi desenvolver um método para determinação de Si em pastilhas de folhas de cana-de-açúcar por espectrometria de emissão óptica com plasma induzido por laser (LIBS). O arranjo experimental foi composto por um laser pulsado de Nd:YAG a 1064 nm (pulsos de 5 ns, 360 mJ, 10 Hz) e os sinais de emissão foram coletados por um telescópio acoplado por fibra óptica ao espectrômetro Echelle com detector ICCD. Amostras laboratoriais consistiram de pastilhas preparadas com folhas de cana-de-açúcar moídas criogenicamente por 40 min. Melhores resultados foram obtidos quando a linha de emissão Si I 212,412 nm foi selecionada e os parâmetros instrumentais foram ajustados em 25 pulsos acumulados...

Multielemental evaluation of garbage bags by EDXRF

Almeida, Eduardo de; Cavagis, Alexandre D. M.; Menegario, Amauri Antonio; Nascimento Filho, Virgilio Franco
Fonte: Taylor & Francis Ltd Publicador: Taylor & Francis Ltd
Tipo: Artigo de Revista Científica Formato: 1113-1122
ENG
Relevância na Pesquisa
45.69%
Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq); Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP); Garbage bags have been broadly used for collecting household waste in Brazil and worldwide. Many of these bags are made from recycled polymers, and the presence of harmful elements is a matter of concern. In this study, an energy dispersive X-ray fluorescence (EDXRF) approach for direct analysis of garbage bags is proposed. The concentrations of K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr and Pb were determined in 14 garbage bags of different brands purchased from local markets in Piracicaba, Sao Paulo State, Brazil. The EDXRF technique proved to be an effective technique for multielemental, environmentally friendly and direct garbage bag monitoring. For most samples, Ca and Ti presented at minor concentration ranges and K, Cr, Mn, Fe, Ni, Cu, Zn and Pb at minor and trace levels. The EDXRF limits of quantification were K: 220; Ca: 112; Ti: 42; Cr: 19; Mn: 13; Fe: 9.2; Ni: 5.7; Cu: 5.3; Zn: 5.2; Br: 12; Rb: 20; Sr: 28 and Pb:17 mu gg(-)(1). The samples had variable thicknesses, with a superficial density variation of 1.5 to 23% among the triplicates. The trueness of the method was checked by analysing the National Institute of Standards and Technology standard reference material SRM2783.

Direct electrochemical analysis of dexamethasone endocrine disruptor in raw natural waters

Oliveira,Thiago M. B. F.; Ribeiro,Francisco W. P.; do Nascimento,Jefferson M.; Soares,Janete E. S.; Freire,Valder N.; Becker,Helena; Lima-Neto,Pedro de; Correia,Adriana N.
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2012 EN
Relevância na Pesquisa
45.64%
This paper describes an electroanalytical methodology using square-wave adsorptive voltammetry, which has been successfully applied for the direct determination of dexamethasone residues in raw natural waters used for the public supply of the Ceará State, Brazil. The obtained detection limits ranged from 7.47 × 10-9 to 1.80 × 10-8 mol L-1 for the three matrices of raw natural waters evaluated. High percentages of average recovery (98.86% ± 0.72), repeatability (0.32% ± 0.05) and reproducibility (0.91% ± 0.20) were obtained in these samples, reaffirming the sensitivity of the procedure. Energy of the LUMO orbitals and Mülliken’s atomic charges were calculated using the functional BLYP/DNP. The theoretical results allied to the diagnostic criteria of the square-wave voltammetry indicate that the dexamethasone redox mechanism is associated to the quasi-reversible and irreversible reduction process of the ketone groups located at C-20 and C-3, respectively.

Direct analysis of cooperativity in multisubunit allosteric proteins

Zandany, Nitzan; Ovadia, Maya; Orr, Irit; Yifrach, Ofer
Fonte: National Academy of Sciences Publicador: National Academy of Sciences
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
45.72%
Allosteric regulation of protein function is a fundamental phenomenon of major importance in many cellular processes. Such regulation is often achieved by ligand-induced conformational changes in multimeric proteins that may give rise to cooperativity in protein function. At the heart of allosteric mechanisms offered to account for such phenomenon, involving either concerted or sequential conformational transitions, lie changes in intersubunit interactions along the ligation pathway of the protein. However, structure–function analysis of such homooligomeric proteins by means of mutagenesis, although it provides valuable indirect information regarding (allosteric) mechanisms of action, it does not define the contribution of individual subunits nor interactions thereof to cooperativity in protein function, because any point mutation introduced into homooligomeric proteins will be present in all subunits. Here, we present a general strategy for the direct analysis of cooperativity in multisubunit proteins that combines measurement of the effects on protein function of all possible combinations of mutated subunits with analysis of the hierarchy of intersubunit interactions, assessed by using high-order double-mutant cycle-coupling analysis. We show that the pattern of high-order intersubunit coupling can serve as a discriminative criterion for defining concerted versus sequential conformational transitions underlying protein function. This strategy was applied to the particular case of the voltage-activated potassium channel protein (Kv) to provide compelling evidence for a concerted all-or-none activation gate opening of the Kv channel pore domain. An direct and detailed analysis of the contribution of high-order intersubunit interactions to cooperativity in the function of an allosteric protein has not previously been presented.

DIRECT ANALYSIS OF SCHISTOSOMA MANSONI POPULATION STRUCTURE USING AGGREGATED INDIVIDUALS FROM LABORATORY STRAINS AND TOTAL FECAL EGG SAMPLING

Blank, Walter A.; Reis, Eliana A. G.; Thiong’o, Fred W.; Braghiroli, Joao F.; Santos, Jarbas M.; Melo, Paulo R. S.; Guimarães, Isabel C. S.; Silva, Luciano K.; Carmo, Theomira M. A.; Reis, Mitermeyer G.; Blanton, Ronald E.
Fonte: PubMed Publicador: PubMed
Tipo: Artigo de Revista Científica
Publicado em /08/2009 EN
Relevância na Pesquisa
45.62%
Many parasite populations are difficult to sample because they are non-uniformly distributed between several host species and are often not easily collected from the living host, limiting sample size and possibly distorting the representation of the population. For the parasite Schistosoma mansoni, we investigated the use of the aggregated eggs found in the stool of infected individuals as a simple and representative sample. Previously, we demonstrated that microsatellite allele frequencies can be accurately estimated from pooled DNA of cloned S. mansoni adults, and we show here that genotyping parasite populations from reproductively isolated laboratory strains can be used to identify these specific populations based on characteristic patterns of allele frequencies, as observed by polyacrylamide gel electrophoresis and automated sequencer analysis of fluorescently labeled PCR products. In addition, microsatellites used to genotype aggregates of eggs collected from stools of infected individuals produced results consistent with the geographic distribution of the samples. Direct analysis of total stool eggs can be an important approach to questions of population genetics for this parasite by increasing the sample size to thousands per individual and reducing bias.

Direct Analysis of Biological Tissue by Paper Spray Mass Spectrometry

Wang, He; Manicke, Nicholas E.; Yang, Qian; Zheng, Lingxing; Shi, Riyi; Cooks, R. Graham; Ouyang, Zheng
Fonte: PubMed Publicador: PubMed
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
45.68%
Paper spray mass spectrometry (PS-MS) is explored as a fast and convenient way for direct analysis of molecules in tissues with minimum sample pretreatment. This technique allows direct detection of different types of molecules such as hormones, lipids and therapeutic drugs in short total analysis times (less than one minute) using a small volume of tissue sample (typically 1 mm3 or less). The tissue sample could be obtained by needle aspiration biopsy, by punch biopsy, or by rubbing a thin tissue section across the paper. There exists potential for the application of paper spray mass spectrometry together with tissue biopsy for clinical diagnostics.

Rapid direct analysis in real time (DART) mass spectrometric detection of juvenile hormone III and its terpene precursors

Navare, Arti T.; Mayoral, Jaime G.; Nouzova, Marcela; Noriega, Fernando G.; Fernández, Facundo M.
Fonte: PubMed Publicador: PubMed
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
45.64%
Direct analysis in real time (DART) is a plasma-based ambient ionization technique that enables rapid ionization of small molecules with high sample throughput. In this work, DART was coupled to an orthogonal (oa) time-of-flight (TOF) mass spectrometer and the system was optimized for analyzing a vital hormonal regulator in insects, juvenile hormone (JH) III and its terpene precursors, namely, farnesol, farnesoic acid, and methyl farne-soate. Optimization experiments were planned using design of experiments (DOE) full factorial models to identify the most significant DART variables contributing to JH III analysis sensitivity by DART-TOF mass spectrometry (MS). The optimized DART-TOF MS method had femto-mole to sub-picomole detection limits for terpene standards, along with mass accuracies below 5 ppm. Finally, the possibility of distinguishing between two farnesol isomers by in-source-collision-induced dissociation (CID) in the first differentially pumped region of the oaTOF mass spectrometer was investigated. DART-MS enabled high-throughput, sensitive analysis with acquisition times ranging from 30 s to a minute. To the best of our knowledge, this is the first report on the application of DART-MS to the detection and identification of volatile or semi-volatile insect terpenoids...

Direct Analysis of Textile Fabrics and Dyes Using IR Matrix-Assisted Laser Desorption Electrospray Ionization (MALDESI) Mass Spectrometry

Cochran, Kristin H.; Barry, Jeremy A.; Muddiman, David C.; Hinks, David
Fonte: PubMed Publicador: PubMed
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
45.75%
The forensic analysis of textile fibers uses a variety of techniques from microscopy to spectroscopy. One such technique that is often used to identify the dye(s) within the fiber is mass spectrometry (MS). In the traditional MS method, the dye must be extracted from the fabric and the dye components are separated by chromatography prior to mass spectrometric analysis. Direct analysis of the dye from the fabric allows the omission of the lengthy sample preparation involved in extraction, thereby significantly reducing the overall analysis time. Herein, a direct analysis of dyed textile fabric was performed using the infrared matrix-assisted laser desorption electrospray ionization (IR-MALDESI) source for MS. In MALDESI, an IR laser with wavelength tuned to 2.94 μm is used to desorb the dye from the fabric sample with the aid of water as the matrix. The desorbed dye molecules are then post-ionized by electrospray ionization (ESI). A variety of dye classes were analyzed from various fabrics with little to no sample preparation allowing for the identification of the dye mass and in some cases the fiber polymer. Those dyes that were not detected using MALDESI were also not observed by direct infusion ESI of the dye standard.

Intact and Top-Down Characterization of Biomolecules and Direct Analysis Using Infrared Matrix-Assisted Laser Desorption Electrospray Ionization Coupled to FT-ICR Mass Spectrometry

Sampson, Jason S.; Murray, Kermit K.; Muddiman, David C.
Fonte: PubMed Publicador: PubMed
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
45.62%
We report the implementation of an infrared laser onto our previously reported matrix-assisted laser desorption electrospray ionization (MALDESI) source with ESI post-ionization yielding multiply charged peptides and proteins. Infrared (IR)-MALDESI is demonstrated for atmospheric pressure desorption and ionization of biological molecules ranging in molecular weight from 1.2 to 17 kDa. High resolving power, high mass accuracy single-acquisition Fourier transform ion cyclotron resonance (FT-ICR) mass spectra were generated from liquid-and solid-state peptide and protein samples by desorption with an infrared laser (2.94 µm) followed by ESI post-ionization. Intact and top-down analysis of equine myoglobin (17 kDa) desorbed from the solid state with ESI post-ionization demonstrates the sequencing capabilities using IR-MALDESI coupled to FT-ICR mass spectrometry. Carbohydrates and lipids were detected through direct analysis of milk and egg yolk using both UV- and IR-MALDESI with minimal sample preparation. Three of the four classes of biological macromolecules (proteins, carbohydrates, and lipids) have been ionized and detected using MALDESI with minimal sample preparation. Sequencing of O-linked glycans, cleaved from mucin using reductive β-elimination chemistry...

Direct Analysis in Real Time Mass Spectrometry (DART-MS) Analysis of Skin Metabolome Changes in the Ultraviolet B-Induced Mice

Park, Hye Min; Kim, Hye Jin; Jang, Young Pyo; Kim, Sun Yeou
Fonte: The Korean Society of Applied Pharmacology Publicador: The Korean Society of Applied Pharmacology
Tipo: Artigo de Revista Científica
Publicado em /11/2013 EN
Relevância na Pesquisa
45.67%
Ultraviolet (UV) radiation is a major environmental factor that leads to acute and chronic reactions in the human skin. UV exposure induces wrinkle formation, DNA damage, and generation of reactive oxygen species (ROS). Most mechanistic studies of skin physiology and pharmacology related with UV-irradiated skin have focused on proteins and their related gene expression or single- targeted small molecules. The present study identified and analyzed the alteration of skin metabolites following UVB irradiation and topical retinyl palmitate (RP, 5%) treatment in hairless mice using direct analysis in real time (DART) time-of-flight mass spectrometry (TOF-MS) with multivariate analysis. Under the negative ion mode, the DART ion source successfully ionized various fatty acids including palmitoleic and linolenic acid. From DART-TOF-MS fingerprints measured in positive mode, the prominent dehydrated ion peak (m/z: 369, M+H-H2O) of cholesterol was characterized in all three groups. In positive mode, the discrimination among three groups was much clearer than that in negative mode by using multivariate analysis of orthogonal partial-least squares-discriminant analysis (OPLS-DA). DART-TOF-MS can ionize various small organic molecules in living tissues and is an efficient alternative analytical tool for acquiring full chemical fingerprints from living tissues without requiring sample preparation. DART-MS measurement of skin tissue with multivariate analysis proved to be a powerful method to discriminate between experimental groups and to find biomarkers for various experiment models in skin dermatological research.

Evaluation of Direct Analysis for Trace Elements in Tea and Herbal Beverages by ICP-MS

Milani,Raquel F.; Morgano,Marcelo A.; Saron,Elisabete S.; Silva,Fabio F.; Cadore,Solange
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/06/2015 EN
Relevância na Pesquisa
65.78%
In general, inductively coupled plasma mass spectrometry (ICP-MS) food analysis requires numerous sample treatment steps that imply an increase of analysis time and the use of chemicals. In this study, the main objective was to evaluate the applicability of the direct analysis by ICP-MS to determine twelve elements (Al, As, Ba, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Se and Zn) in tea and herbal beverages. Direct analysis method was compared with two other sample treatments: minimum treatment (acid dilution) and using a destructive method (microwave assisted digestion). Besides the lowest time of analysis, direct analysis provides a reliable response and agrees with the “green chemistry” principles. High sensitivity was also observed by low values of limits of detection and quantification, in general, below 2.5 µg L-1. The method accuracy was evaluated by spiked experiments and values ranged between 82 and 120%. Low values of coefficient of variation were also observed, 2 to 17%, for all analytes. The method exhibited applicability for commercial tea samples as well as for drinks made by herb infusion.

Analysis of Synthetic Cannabinoids by Direct Analysis in Real Time Quadrupole Time-of-Flight Mass Spectrometry and Gas Chromatography Quadrupole Time-of-Flight Mass Spectrometry

Torbet, Tyler S
Fonte: FIU Digital Commons Publicador: FIU Digital Commons
Tipo: Artigo de Revista Científica Formato: application/pdf
Relevância na Pesquisa
65.76%
The aim of this study was to investigate the utility of direct analysis in real time quadrupole time-of-flight mass spectrometry and gas chromatography quadrupole time-of-flight mass spectrometry in the analysis of 162 different synthetic cannabinoids. Direct analysis in real time quadrupole time-of-flight mass spectrometry is shown to be a rapid and accurate analytical method for synthetic cannabinoids. Spectra can be generated with less than 1.5 ng of the drug in under a minute and be successfully searched against previously generated ESI-QTOF libraries in most cases (118/130 drugs tested) as well as can also be applied to the identification of synthetic cannabinoids in a mixture. Gas chromatography quadrupole time-of-flight mass spectrometry, while requiring a much longer analysis time, is shown to accurately distinguish all but 19 compounds (140/159). These two instruments have proven to be viable alternatives in synthetic cannabinoid analysis and will greatly benefit forensic laboratories.

Evaluation of different sample preparation procedures using chemometrics: comparison among photo-fenton reaction, microwave irradiation, and direct determination of minerals in fruit juices.

GROMBONI, C. F.; CARAPELLI, R.; FEREIRA FILHO, E. R.; NOGUEIRA, A. R. de A.
Fonte: Food Analytical Methods, v. 3, p. 98-103, 2010. Publicador: Food Analytical Methods, v. 3, p. 98-103, 2010.
Tipo: Artigo em periódico indexado (ALICE)
PT_BR
Relevância na Pesquisa
45.69%
In this work, an exploratory study about the mineral characteristic of some fruit juice (passion fruit, pineapple, orange, and grape) applying chemometric tools was made. The juices analyzed were separated in different groups by principal components analysis and hierarchical components analysis in accordance with their minerals contents. Barium, C, Ca, K, Mg, Mn, Na, and Sr were determined by inductively coupled plasma optical emission spectrometry. Addition and recovery methods were used for confirmation of the results. The recovery range for microwave sample preparation was from 81% (for K) to 111% (for Mn), for photo-Fenton from 102% (for Ca e Mg) to 128% (for Na), and the direct analysis, without sample preparation step, from 96% (for K) to 139% (for Mn). A new method based on photo-Fenton reaction coupled with microwave radiation for juice decomposition was proposed; the obtained results were satisfactory and compatible with the conventional methods of analysis in accordance with Student's statistic t test and chemometric tools.; 2010

Simultaneous determination of 3-chlorotyrosine and 3-nitrotyrosine in human plasma by direct analysis in real time–tandem mass spectrometry

Song, Yuqiao; Liao, Jie; Zha, Cheng; Wang, Bin; Liu, Charles C.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
45.64%
A novel method for the simultaneous determination of 3-nitrotyrosine (NT) and 3-chlorotyrosine (CT) in human plasma has been developed based on direct analysis in real time–tandem mass spectrometry (DART–MS/MS). Analysis was performed in the positive ionization mode using multiple reaction monitoring (MRM) of the ion transitions at m/z 216.2/170.1 for CT, m/z 227.2/181.1 for NT and m/z 230.2/184.2 for the internal standard, d3-NT. The assay was linear in the ranges 0.5–100 μg/mL for CT and 4–100 μg/mL for NT with corresponding limits of detection of 0.2 and 2 μg/mL. Intra- and inter-day precisions and accuracies were respectively <15% and ±15%. Matrix effects were also evaluated. The method is potentially useful for high throughput analysis although sensitivity needs to be improved before it can be applied in clinical research.

Cuticular hydrocarbon analysis of an awake behaving fly using direct analysis in real-time time-of-flight mass spectrometry

Yew, Joanne Y.; Cody, Robert B.; Kravitz, Edward A.
Fonte: National Academy of Sciences Publicador: National Academy of Sciences
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
45.66%
In mammals and insects, pheromones strongly influence social behaviors such as aggression and mate recognition. In Drosophila melanogaster, pheromones in the form of cuticular hydrocarbons play prominent roles in courtship. GC/MS is the primary analytical tool currently used to study Drosophila cuticular hydrocarbons. Although GC/MS is highly reproducible and sensitive, it requires that the fly be placed in a lethal solution of organic solvent, thereby impeding further behavioral studies. We present a technique for the analysis of hydrocarbons and other surface molecules from live animals by using direct analysis in real-time (DART) MS. Cuticular hydrocarbons were sampled from the surface of a restrained, awake behaving fly by using several brief, carefully controlled depressions of the abdomen with a small steel probe. DART mass spectral analysis of the probe detected ions with mass-to-charge ratio (m/z) of the protonated molecule corresponding to many of the previously identified unsaturated hydrocarbons. Six additional cuticular hydrocarbons also were identified. Consistent with previous GC/MS studies, male and female differences in chemical composition were evident. Spatial differences in the expression profile also were observed on males. Sampling from an individual female first as a virgin and then 45 and 90 min after successful copulation showed that mass signals likely to correspond to cis-vaccenyl acetate...

Assessment of Direct Mercury Analyzer® to quantify mercury in soils and leaf samples

Melendez-Perez,Jose J.; Fostier,Anne H.
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/11/2013 EN
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This work aims to assess a method for total Hg quantification in soil and leaf samples by using a Direct Mercury Analyzer® (DMA-80 TRICELL; Milestone Inc., Italy). Standard Reference materials of tree leaves, river sediment and soil, and collected samples of soil and leaves were used to optimize and to validate the method. Given that the technique allows direct analysis of samples by combustion, aspects like effect of sample amount variation and sample granulometry were considered. Method's robustness was also assessed through the Youden test showing that for leaf sample analyses, among the seven tested factors, four were able to significantly affect the analytical results, but the soil samples results were not significantly affected by slight variations of any of the seven factors. Recoveries for reference materials ranged from 102% to 104%, and the precision (RSD) was lower than 5%.