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Evaluation of comprehensive two-dimensional gas chromatography coupled to rapid scanning quadrupole mass spectrometry for quantitative analysis

Goncalves Silva, Bruno Jose; Tranchida, Peter Quinto; Purcaro, Giorgia; Costa Queiroz, Maria Eugenia; Mondello, Luigi; Lanças, Fernando Mauro
Fonte: ELSEVIER SCIENCE BV; AMSTERDAM Publicador: ELSEVIER SCIENCE BV; AMSTERDAM
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
76.04%
Comprehensive two-dimensional gas chromatography (GC x GC) is a powerful technique that provides excellent separation and identification of analytes in highly complex samples with considerable increase in GC peak capacities. However, since second dimension analyses are very fast, detectors with a rapid acquisition rate are required. Over the last years, quite a number of studies have discussed the potential and limitations of the combination GC x GC with a variety of quadrupole mass spectrometers. The present research focuses on the evaluation of qMS effectiveness at a 10,000-amu/s scan speed and 20-Hz scan frequency for the identification (full scan mode acquisition-TIC) and quantification (extracted ion chromatogram) of target pesticide residues in tomato samples. The following MS parameters have been evaluated: number of data points per peak, mass spectrum quality, peak skewing, and sensitivity. The validated proposed GC x GC/qMS method presented satisfactory results in terms of repeatability (coefficient of variation lower than 15%), accuracy (84-117%), and linearity (ranging from 25 to 500 ng/g), while significant enhancement in sensitivity was observed (a factor of around 10) under scan conditions. (C) 2012 Elsevier B.V. All rights reserved.

Determination of disease biomarkers in Eucalyptus by comprehensive two-dimensional gas chromatography and multivariate data analysis

Hantao, Leandro Wang; Aleme, Helga Gabriela; Passador, Martha Maria; Furtado, Edson Luiz; Ribeiro, Fabiana Alves de Lima; Poppi, Ronei Jesus; Augusto, Fabio
Fonte: Universidade Estadual Paulista Publicador: Universidade Estadual Paulista
Tipo: Artigo de Revista Científica Formato: 86-91
ENG
Relevância na Pesquisa
86.19%
In this paper is reported the use of the chromatographic profiles of volatiles to determine disease markers in plants - in this case, leaves of Eucalyptus globulus contaminated by the necrotroph fungus Teratosphaeria nubilosa. The volatile fraction was isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography-fast quadrupole mass spectrometry (GC. ×. GC-qMS). For the correlation between the metabolic profile described by the chromatograms and the presence of the infection, unfolded-partial least squares discriminant analysis (U-PLS-DA) with orthogonal signal correction (OSC) were employed. The proposed method was checked to be independent of factors such as the age of the harvested plants. The manipulation of the mathematical model obtained also resulted in graphic representations similar to real chromatograms, which allowed the tentative identification of more than 40 compounds potentially useful as disease biomarkers for this plant/pathogen pair. The proposed methodology can be considered as highly reliable, since the diagnosis is based on the whole chromatographic profile rather than in the detection of a single analyte. © 2013 Elsevier B.V..

Evidence for euphotic zone anoxia during the deposition of Aptian source rocks based on aryl isoprenoids in petroleum, Sergipe-Alagoas Basin, northeastern Brazil

Sousa Júnior, Gustavo R.; Santos, AntÔnia L.S.; De Lima, Sidney G.; Lopes, José A.D.; Reis, Francisco A.M.; Santos Neto, Eugênio V.; Chang, Hung K.
Fonte: Universidade Estadual Paulista Publicador: Universidade Estadual Paulista
Tipo: Artigo de Revista Científica Formato: 94-104
ENG
Relevância na Pesquisa
106.2%
Four crude oil samples from the Sergipe-Alagoas Basin, northeastern Brazil, were analyzed using full scan gas chromatography-quadrupole mass spectrometry (GC-qMS) for biomarkers, in order to correlate them using aromatic carotenoids thereby enhancing knowledge about the depositional environment of their source rocks. The geochemical parameters derived from saturated fractions of the oils show evidence of little or no biodegradation and similar thermal maturation (Ts/(Ts+Tm) for terpanes, C29 αββ/(αββ+ααα), C27, and C29 20S/(20S+20R) for steranes). Low pristane/phytane ratios and the abundance of gammacerane and β-carotane are indicative of an anoxic and saline depositional environment for the source rocks. Moreover, we identified a large range of diagenetic and catagenetic products of the aromatic carotenoid isorenieratene, including C40, C33, and C32 diaryl isoprenoids and aryl isoprenoid derivatives with short side chains and/or additional rings. These results indicate anoxia in the photic zone during the deposition of the source rocks. © 2013 The Authors.

Comprehensive two-dimensional gas chromatography combined to multivariate data analysis for detection of disease-resistant clones of Eucalyptus

Hantao, Leandro Wang; Toledo, Bruna Regina; Lima Ribeiro, Fabiana Alves de; Pizetta, Marilia; Pierozzi, Caroline Geraldi; Furtado, Edson Luiz; Augusto, Fabio
Fonte: Elsevier B.V. Publicador: Elsevier B.V.
Tipo: Artigo de Revista Científica Formato: 1079-1084
ENG
Relevância na Pesquisa
76%
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP); Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq); Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES); In this paper it is reported the use of the chromatographic profiles from volatile fractions of plant clones - in this case, hybrids of Eucalyptus grandis x Eucalyptus urophylla - to determine specimens susceptible to rust disease. The analytes were isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography combined to fast quadrupole mass spectrometry (GC x GC-qMS). Parallel Factor Analysis (PARAFAC) was employed for estimate the correlation between the chromatographic profiles and resistance against Eucalyptus rust, after preliminary variable selection performed by Fisher ratio analysis. The proposed method allowed the differentiation between susceptible and non-susceptible clones and determination of three resistance biomarkers. This approach can be a valuable alternative for the otherwise time-consuming and laborintensive methods commonly used. (C) 2013 Elsevier B.V. All rights reserved.

Microextração em fase sólida e cromatografia gasosa convencional e bidimensional para classificação de méis; Solid phase microextraction and conventional and comprehensive gas chromatography for the classification of honeys

Sandra Regina Rivellino Marques
Fonte: Biblioteca Digital da Unicamp Publicador: Biblioteca Digital da Unicamp
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 17/11/2011 PT
Relevância na Pesquisa
75.96%
A técnica de microextração em fase sólida através do headspace (HS-SPME) combinada com a cromatografia gasosa bidimensional abrangente e detecção por ionização em chama (GCxGCxFID) foi empregada para detectar artefatos formados durante o preparo da amostra de méis, que poderiam ser prejudiciais ao processo de identificação de sua origem floral. O método foi otimizado utilizando-se planejamento multivariado. Para isso, uma mistura de diferentes tipos de méis brasileiros foi usada como modelo. Os artefatos de extração identificados foram classificados como resultantes da manipulação através do HS. A influência da temperatura e do tempo de exposição ao tratamento térmico também foi avaliada. A identificação da fração volátil da mistura de mel foi realizada por GCxGCxFID e cromatografia gasosa acoplada à espectrometria de massas com analisador quadrupolar (GC-QMS) comparando-se o índice de retenção linear com programação de temperatura obtido na primeira dimensão (D-LTPRI), calculado a partir dos cromatogramas obtidos por GCxGCxFID, e os índices obtidos por GC-QMS para as mesmas amostras. Esta identificação foi confirmada por cromatografia gasosa bidimensional abrangente combinada a um espectrômetro de massas por tempo de vôo (GCxGCxTOFMS). Portanto...

Characterization of the volatile fraction emitted by phloems of four pinus species by solid-phase microextraction and gas chromatography–mass spectrometry

Santos, A.M.; Vasconcelos, T.; Mateus, E.; Farrall, M.H.; Silva, M. D. R. Gomes da; Paiva, Maria Rosa; Branco, M.
Fonte: Journal of Chromatography A Publicador: Journal of Chromatography A
Tipo: Artigo de Revista Científica
Publicado em //2006 ENG
Relevância na Pesquisa
56%
Pine forests constitute some of the most important renewable resources supplying timber, paper and chemical industries, among other functions. Characterization of the volatiles emitted by different Pinus species has proven to be an important tool to decode the process of host tree selection by herbivore insects, some of which cause serious economic damage to pines. Variations in the relative composition of the bouquet of semiochemicals are responsible for the outcome of different biological processes, such as mate finding, egg-laying site recognition and host selection. The volatiles present in phloem samples of four pine species, P. halepensis, P. sylvestris, P. pinaster and P. pinea, were identified and characterized with the aim of finding possible host-plant attractants for native pests, such as the bark beetle Tomicus piniperda. The volatile compounds emitted by phloem samples of pines were extracted by headspace solid-phase micro extraction, using a 2 cm 50/30 mm divinylbenzene/carboxen/polydimethylsiloxane table flex solid-phase microextraction fiber and its contents analyzed by high-resolution gas chromatography, using flame ionization and a non polar and chiral column phases. The components of the volatile fraction emitted by the phloem samples were identified by mass spectrometry using time-of-flight and quadrupole mass analyzers. The estimated relative composition was used to perform a discriminant analysis among pine species...

Liquid chromatography - tandem quadrupole mass spectrometry and comprehensive two-dimensional gas chromatography - time-of-flight mass spectrometry measurement of targeted metabolites of Methylobacterium extorquens AM1 grown on two different carbon sources

Yang, Song; Sadilek, Martin; Synovec, Robert E.; Lidstrom, Mary E.
Fonte: PubMed Publicador: PubMed
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
66.19%
Complementary methods using liquid chromatography - tandem quadrupole mass spectrometry (LC-MS/MS) and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOF-MS) were developed and applied to determine targeted metabolites involved in central carbon metabolism [including tricarboxylic acid cycle, serine cycle, ethylmalonyl-coenzyme A (ethylmalonyl-CoA) pathway and poly-β-hydroxybutyrate cycle] of the bacterium Methylobacterium extorquens AM1 grown on two carbon sources, ethylamine (C2) and succinate (C4). Nucleotides, acyl-CoAs and a few volatile metabolites in cell extracts of M. extorquens AM1 were readily separated using either hydrophilic interaction liquid chromatography or reversed-phase liquid chromatography, and detected with good sensitivity by MS/MS. However, volatile intermediates within a low mass range (<300 m/z), especially at low abundance (such as glyoxylic acid and others <500 nM), were more effectively analyzed by GC × GC-TOF-MS which often provided better sensitivity, resolution and reproducibility. The complementary nature of the LC-based and GC-based methods allowed the comparison of 39 metabolite concentrations (the lowest level was at 139.3 nM). The overlap between the LC and GC-based methods of 7 metabolites provided a basis to check for consistency between the two methods...

Streamlined pentafluorophenylpropyl column liquid chromatography-tandem quadrupole mass spectrometry and global 13C-labeled internal standards improve performance for quantitative metabolomics in bacteria

Yang, Song; Sadilek, Martin; Lidstrom, Mary E.
Fonte: PubMed Publicador: PubMed
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
66.03%
Streamlined quantitative metabolomics in central metabolism of bacteria would be greatly facilitated by a high-efficiency liquid chromatography (LC) method in conjunction with accurate quantitation. To achieve this goal, a methodology for LC-tandem quadrupole mass spectrometry (LC-MS/MS) involving a pentafluorophenylpropyl (PFPP) column and culture-derived global 13C-labeled internal standards (I.Ss.) has been developed and compared to hydrophilic interaction liquid chromatography (HILIC)-MS/MS and published combined two-dimensional gas chromatography and LC methods. All 50 tested metabolite standards from 5 classes (amino acids, carboxylic acids, nucleotides, acyl-CoAs and sugar phosphates) displayed good chromatographic separation and sensitivity on the PFPP column. In addition, many important critical pairs such as isomers / isobars (e.g. isoleucine / leucine, methylsuccinic acid / ethylmalonic acid and malonyl-CoA / 3-hydroxybutyryl-CoA) and metabolites of similar structure (e.g. malate / fumarate) were resolved better on the PFPP than on the HILIC column. Compared to only one 13C-labeled I.S., the addition of global 13C-labeled I.Ss. improved quantitative linearity and accuracy. PFPP-MS/MS with global 13C-labeled I.Ss. allowed the absolute quantitation of 42 metabolite pool sizes in M. extorquens AM1. A comparison of metabolite level changes published previously for ethylamine (C2) versus succinate (C4) cultures of Methylobacterium extorquens AM1 indicated a good consistency with the data obtained by PFPP-MS/MS...

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
96.35%
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.

Screening of volatile composition from portuguese multifloral honeys using headspace solid-phase microextraction-gas chromatography–quadrupole mass spectrometry

Pontes, M.; Marques, J. C.; Câmara, J. S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /11/2007 ENG
Relevância na Pesquisa
106.03%
The volatile composition from four types of multifloral Portuguese (produced in Madeira Island) honeys was investigated by a suitable analytical procedure based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography–quadrupole mass spectrometry detection (GC–qMS). The performance of five commercially available SPME fibres: 100 μm polydimethylsiloxane, PDMS; 85 μm polyacrylate, PA; 50/30 μm divinylbenzene/carboxen on polydimethylsiloxane, DVB/CAR/PDMS (StableFlex); 75 μm carboxen/polydimethylsiloxane, CAR/PDMS, and 65 μm carbowax/divinylbenzene, CW/DVB; were evaluated and compared. The highest amounts of extract, in terms of the maximum signal obtained for the total volatile composition, were obtained with a DVB/CAR/PDMS coating fibre at 60 °C during an extraction time of 40 min with a constant stirring at 750 rpm, after saturating the sample with NaCl (30%). Using this methodology more than one hundred volatile compounds, belonging to different biosynthetic pathways were identified, including monoterpenols, C13-norisoprenoids, sesquiterpenes, higher alcohols, ethyl esters and fatty acids. The main components of the HS-SPME samples of honey were in average ethanol, hotrienol...

Comparative analysis of the volatile fraction from Annona cherimola Mill. cultivars by solid-phase microextraction and gas chromatography–quadrupole mass spectrometry detection

Ferreira, Liseth; Perestrelo, Rosa; Câmara, J. S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /01/2009 ENG
Relevância na Pesquisa
106.03%
The analysis of volatile compounds in Funchal, Madeira, Mateus and Perry Vidal cultivars of Annona cherimola Mill. (cherimoya) was carried out by headspace solid-phase microextraction (HS-SPME) combined with gas chromatography–quadrupole mass spectrometry detection (GC–qMSD). HS-SPME technique was optimized in terms of fibre selection, extraction time, extraction temperature and sample amount to reach the best extraction efficiency. The best result was obtained with 2 g of sample, using a divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fibre for 30 min at 30 °C under constant magnetic stirring (800 rpm). After optimization of the extraction methodology, all the cherimoya samples were analysed with the best conditions that allowed to identify about 60 volatile compounds. The major compounds identified in the four cherimoya cultivars were methyl butanoate, butyl butanoate, 3-methylbutyl butanoate, 3-methylbutyl 3-methylbutanoate and 5-hydroxymethyl-2-furfural. These compounds represent 69.08 ± 5.22%, 56.56 ± 15.36%, 56.69 ± 9.28% and 71.82 ± 1.29% of the total volatiles for Funchal, Madeira, Mateus and Perry Vidal cultivars, respectively. This study showed that each cherimoya cultivars have 40 common compounds...

Profiling allergic asthma volatile metabolic patterns using a headspace-solid phase microextraction/gas chromatography based methodology

Caldeira, M.; Barros, A. S.; Bilelo, M. J.; Parada, A.; Câmara, J. S.; Rocha, S. M.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /06/2011 ENG
Relevância na Pesquisa
96%
Allergicasthmarepresentsanimportantpublichealthissuewithsignificantgrowthovertheyears,especially in the paediatric population. Exhaled breath is a non-invasive, easily performed and rapid method forobtainingsamplesfromthelowerrespiratorytract.Inthepresentmanuscript,themetabolicvolatile profiles of allergic asthma and control children were evaluated by headspace solid-phase microextraction combined with gas chromatography–quadrupole mass spectrometry (HS-SPME/GC–qMS). The lack ofstudiesinbreathofallergicasthmaticchildrenbyHS-SPMEledtothedevelopmentofanexperimental design to optimize SPME parameters. To fulfil this objective, three important HS-SPME experimental parameters that influence the extraction efficiency, namely fibre coating, temperature and time extractions were considered. The selected conditions that promoted higher extraction efficiency corresponding to the higher GC peak areas and number of compounds were: DVB/CAR/PDMS coating fibre, 22◦C and 60min as the extraction temperature and time, respectively. The suitability of two containers, 1L Tedlar® bags and BIOVOC®, for breath collection and intra-individual variability were also investigated. The developed methodology was then applied to the analysis of children exhaled breath with allergicasthma(35)...

Mass spectrometry for identifying pharmaceutical biotransformation products in the environment

Kosjek, T.; Heath, E.; Petrovic, Mira; Barceló, Damià
Fonte: Elsevier Publicador: Elsevier
Tipo: Artículo Formato: 162 bytes; application/msword
ENG
Relevância na Pesquisa
66.03%
9 pages, 2 figures, 1 table.-- Printed version published Dec 2007.-- Issue title: Emerging contaminants in wastewaters.; Many classes of pharmaceuticals have been detected in wastewaters and surface waters around Europe, but little is known about their occurrence, fate and potential harmful effects on the environment, and that makes them an important group among those compounds considered to be new emerging contaminants. To understand the cycling of pharmaceuticals and their metabolites, it is essential to possess qualitative and quantitative information on their presence in the environment. This review covers the current status and future prospects of advanced hyphenated mass spectrometric (MS) techniques (gas chromatography-MS (GC-MS) and liquid chromatography-MS (LC-MS)) in elucidating the structures of trace contaminants, namely pharmaceutical biodegradation products in complex environmental matrices. The article is oriented towards technique and method and discusses capabilities, potential and limitations of different GC and LC mass analyzers (quadrupole, ion trap, time-of-flight and hybrid techniques) in dealing with analytical challenges of complex matrices and trace contaminants. We also give practical examples of their applications. The main scope of this article is to support and to facilitate the on-going research on pharmaceutical biodegradation products in environmental samples.; This work was performed with the financial support of Ad futura fellowship (Science and Education Foundation of the Republic of Slovenia...

Optimization of quadrupole ion storage mass spectrometric conditions for the analysis of selected polybrominated diphenyl ethers. Comparative approach with negative chemical ionization and electron impact mass spectrometry

Larrazábal, David; Martínez, M. Ángeles; Eljarrat, Ethel; Barceló, Damià; Fabrellas, Begoña
Fonte: John Wiley & Sons Publicador: John Wiley & Sons
Tipo: Artículo Formato: 22195 bytes; application/pdf
ENG
Relevância na Pesquisa
66.02%
8 pages, 4 figures, 3 tables.-- PMID: 15468104 [PubMed].; Gas chromatography coupled to quadrupole ion storage mass spectrometry (QISTMS) operating in the non-resonant mode is presented as an innovative approach for the analysis of selected polybrominated diphenyl ethers (PBDEs). Although reductions in complexity and time needed for optimization are achieved in comparison with the resonant option, precise adjustment of the mass spectrometric conditions is required. Differences in isolation and fragmentation patterns of target species with degree of bromination were observed. The reliability of the method was confirmed by using standard solutions through the evaluation of certain quality parameters such as accuracy (92-108%), injection repeatability and reproducibility (coefficient of variation below 10% and 15%, respectively). Detection limits ranged from 62 to 621 fg, providing sensitivity similar to that of negative chemical ionisation (NCIMS) and greater than that of electron ionization mass spectrometry. The applicability of QISTMS method to real samples and matrix effects were evaluated through the analysis of some PBDE congeners in a sewage sludge sample from a Spanish waste-water treatment plant. Comparable results were obtained using QISTMS and NCIMS. According to these observations...

Characterization and Quantification of Isoprene-Derived Epoxydiols in Ambient Aerosol in the Southeastern United States

Chan, Man Nin; Surratt, Jason D.; Claeys, Magda; Edgerton, Eric S.; Tanner, Roger L.; Shaw, Stephanie L.; Zheng, Mei; Knipping, Eladio M.; Eddingsaas, Nathan C.; Wennberg, Paul O.; Seinfeld, John H.
Fonte: American Chemical Society Publicador: American Chemical Society
Tipo: Article; PeerReviewed Formato: application/pdf
Publicado em 15/06/2010
Relevância na Pesquisa
56.02%
Isoprene-derived epoxydiols (IEPOX) are identified in ambient aerosol samples for the first time, together with other previously identified isoprene tracers (i.e., 2-methyltetrols, 2-methylglyceric acid, C5-alkenetriols, and organosulfate derivatives of 2-methyltetrols). Fine ambient aerosol collected in downtown Atlanta, GA and rural Yorkville, GA during the 2008 August Mini-Intensive Gas and Aerosol Study (AMIGAS) was analyzed using both gas chromatography/quadrupole mass spectrometry (GC/MS) and gas chromatography/time-of-flight mass spectrometry (GC/TOFMS) with prior trimethylsilylation. Mass concentrations of IEPOX ranged from ~1 to 24 ng m^(−3) in the aerosol collected from the two sites. Detection of particle-phase IEPOX in the AMIGAS samples supports recent laboratory results that gas-phase IEPOX produced from the photooxidation of isoprene under low-NO_x conditions is a key precursor of ambient isoprene secondary organic aerosol (SOA) formation. On average, the sum of the mass concentrations of IEPOX and the measured isoprene SOA tracers accounted for about 3% of the organic carbon, demonstrating the significance of isoprene oxidation to the formation of ambient aerosol in this region.

Headspace solid-phase microextraction-gas chromatography-quadrupole mass spectrometric methodology for the establishment of the volatile composition of Passiflora fruit species

Pontes, M.; Marques, J. C.; Câmara, J. S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /09/2009 ENG
Relevância na Pesquisa
95.97%
Dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography-quadrupole mass spectrometry analysis (GC-qMS), was used to investigate the aroma profile of different species of passion fruit samples. The performance of five commercially available SPME fibres: 65 μm polydimethylsiloxane/divinylbenzene, PDMS/DVB; 100 μm polydimethylsiloxane, PDMS; 85 μm polyacrylate, PA; 50/30 μm divinylbenzene/carboxen on polydimethylsiloxane, DVB/CAR/PDMS (StableFlex); and 75 μm carboxen/polydimethylsiloxane, CAR/PDMS; was evaluated and compared. Several extraction times and temperature conditions were also tested to achieve optimum recovery. The SPME fibre coated with 65 μm PDMS/DVB afforded the highest extraction efficiency, when the samples were extracted at 50 °C for 40 min with a constant stirring velocity of 750 rpm, after saturating the sample with NaCl (17%, w/v — 0.2 g). A comparison among different passion fruit species has been established in terms of qualitative and semi-quantitative differences in volatile composition. By using the optimal extraction conditions and GC-qMS it was possible to tentatively identify seventy one different compounds in Passiflora species: 51 volatiles in Passiflora edulis Sims (purple passion fruit)...

Potentialities of two solventless extraction approaches—Stir bar sorptive extraction and headspace solid-phase microextraction for determination of higher alcohol acetates, isoamyl esters and ethyl esters in wines

Perestrelo, R.; Nogueira, J. M. F.; Câmara, J. S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /12/2009 ENG
Relevância na Pesquisa
106.03%
A stir bar sorptive extraction with liquid desorption followed by large volume injection coupled to gas chromatography–quadrupole mass spectrometry (SBSE-LD/LVI-GC–qMS) was evaluated for the simultaneous determination of higher alcohol acetates (HAA), isoamyl esters (IsoE) and ethyl esters (EE) of fatty acids. The method performance was assessed and compared with other solventless technique, the solid-phase microextraction (SPME) in headspace mode (HS). For both techniques, influential experimental parameters were optimised to provide sensitive and robust methods. The SBSE-LD/LVI methodology was previously optimised in terms of extraction time, influence of ethanol in the matrix, liquid desorption (LD) conditions and instrumental settings. Higher extraction efficiency was obtained using 60 min of extraction time, 10% ethanol content, n-pentane as desorption solvent, 15 min for the back-extraction period, 10 mL min−1 for the solvent vent flow rate and 10 °C for the inlet temperature. For HS-SPME, the fibre coated with 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) afforded highest extraction efficiency, providing the best sensitivity for the target volatiles, particularly when the samples were extracted at 25 °C for 60 min under continuous stirring in the presence of sodium chloride (10% (w/v)). Both methodologies showed good linearity over the concentration range tested...

Optimisation of stir bar sorptive extraction and liquid desorption combined with large volume injection-gas chromatography–quadrupole mass spectrometry for the determination of volatile compounds in wines

Coelho, Elisabete; Perestrelo, Rosa; Neng, Nuno R.; Câmara, José S.; Coimbra, Manuel A.; Nogueira, J. M. F.; Rocha, Sílvia M.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /06/2008 ENG
Relevância na Pesquisa
156.17%
Stir bar sorptive extraction and liquid desorption followed by large volume injection coupled to gas chromatography–quadrupole mass spectrometry (SBSE–LD/LVI-GC–qMS) had been applied for the determination of volatiles in wines. The methodology was optimised in terms of extraction time and influence of ethanol in the matrix; LD conditions, and instrumental settings. The optimisation was carried out by using 10 standards representative of the main chemical families of wine, i.e. guaiazulene, E,E-farnesol, β-ionone, geranylacetone, ethyl decanoate, β-citronellol, 2-phenylethanol, linalool, hexyl acetate and hexanol. The methodology shows good linearity over the concentration range tested, with correlation coefficients higher than 0.9821, a good reproducibility was attained (8.9–17.8%), and low detection limits were achieved for nine volatile compounds (0.05–9.09 μg L−1), with the exception of 2-phenylethanol due to low recovery by SBSE. The analytical ability of the SBSE–LD/LVI-GC–qMS methodology was tested in real matrices, such as sparkling and table wines using analytical curves prepared by using the 10 standards where each one was applied to quantify the structurally related compounds. This methodology allowed, in a single run...

Optimisation of solid-phase microextraction combined with gas chromatography–mass spectrometry based methodology to establish the global volatile signature in pulp and skin of Vitis vinifera L. grape varieties

Perestrelo, Rosa; Barros, António S.; Rocha, Sílvia M.; Câmara, José S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /09/2011 ENG
Relevância na Pesquisa
75.95%
The volatiles (VOCs) and semi-volatile organic compounds (SVOCs) responsible for aroma are mainly present in skin of grape varieties. Thus, the present investigation is directed towards the optimisation of a solvent free methodology based on headspace-solid-phase microextraction (HS-SPME) combined with gas chromatography–quadrupole mass spectrometry (GC–qMS) in order to establish the global volatile composition in pulp and skin of Bual and Bastardo Vitis vinifera L. varieties. A deep study on the extraction-influencing parameters was performed, and the best results, expressed as GC peak area, number of identified compounds and reproducibility, were obtained using 4 g of sample homogenised in 5 mL of ultra-pure Milli-Q water in a 20 mL glass vial with addition of 2 g of sodium chloride (NaCl). A divinylbenzene/carboxen/polydimethylsiloxane fibre was selected for extraction at 60 °C for 45 min under continuous stirring at 800 rpm. More than 100 VOCs and SVOCs, including 27 monoterpenoids, 27 sesquiterpenoids, 21 carbonyl compounds, 17 alcohols (from which 2 aromatics), 10 C13 norisoprenoids and 5 acids were identified. The results showed that, for both grape varieties, the levels and number of volatiles in skin were considerably higher than those observed in pulp. According to the data obtained by principal component analysis (PCA)...

Improved sensitivity using liquid chromatography mass spectrometry (LC-MS) for detection of propyl chloroformate derivatised β-N-methylamino-L-alanine (BMAA) in cyanobacteria

Esterhuizen-Londt,M; Downing,S; Downing,TG
Fonte: Water SA Publicador: Water SA
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/04/2011 EN
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β-N-methylamino-L-alanine (BMAA) is a difficult molecule to detect, primarily due to its presence in low concentrations in complex matrices. This has resulted in contradictory reports on the presence of BMAA in cyanobacteria. We report improved sensitivity of detection using propyl chloroformate derivatisation, liquid chromatographic (LC) separation, and single quadrupole mass spectrometry (MS) detection. Triple quadrupole mass spectrometry (MS/MS) was used to confirm the identity of BMAA in cyanobacteria based on product ions. We show a 10-fold increase in sensitivity with the LC-MS method compared to the previously published gas chromatography mass spectrometry (GC-MS) method with pre-column derivatised BMAA using a commercially available amino acid derivatisation kit. Clear chromatographic separation of BMAA from 2,4-diaminobutyric acid (DAB), as well as the 20 standard amino acids, was achieved. The analytical method was validated by multiple derivatisation of samples, multiple users, and multiple injections, as well as in various matrices. The quantifier ion used was [M + H]+ = 333 m/z. The MS/MS product ions 273 m/z and 245 m/z were used in identification and peak confirmation. Additionally, we confirm the presence of BMAA in cyanobacteria previously screened with GC-MS as well as the presence of BMAA in newly isolated cultures.