HS-SPME Dotaz Zobrazit nápovědu
Volatile aromatic compounds have a major impact on the final organoleptic properties of cider, and their profiles are influenced by a number of parameters that are closely related to production technologies, especially with regard to the raw material, the microorganism used and the fermentation process. In this work, the profiles of volatile compounds (4 fatty acids, 6 higher alcohols and 12 esters) from 34 European ciders were studied using HS-SPME-GC-MS. Volatiles were isolated by HS-SPME using a CAR/PDMS fiber. Analytical data were statistically evaluated using principal component analysis, and differences in composition of volatiles between cider produced using "intensified" technologies and that of ciders produced by traditional production processes were demonstrated. This difference was mainly due to varying contents of some higher alcohols (2-methylpropanol, isoamyl alcohols, hexanol, and butane-2,3-diol) and esters (ethyl 2-methylbutanoate, butylacetate, and hexyl acetate).
Headspace solid-phase microextraction (HS-SPME) and solid-phase microextraction coupled with hydrodistillation (HD-SPME) were used for detection and determination of essential oils in dried leaves of Mentha piperita L., Lavandula augustifolia L. and Salvia officinalis L. The results were compared with those obtained using steam distillation, which is a reference method. The extraction time 15 min and the minimal fibre depth 1.4 cm are suitable for a 50/30 ?m polydimethylsiloxane/divinylbenzene/ carboxen fibre. The method was compared with HS-SPME and steam distillation.
A new method has been developed to detect 36 pesticides that may contaminate tea samples (green, black and fruit tea). The hyphenation of solid-phase microextraction in head-space mode with a comprehensive two-dimensional gas chromatography coupled with high-speed time-of-flight mass spectrometry (HS-SPME-GCxGC/TOF MS) proved to be a quick alternative to conventional GC/MS methodology which employs solvent-based extraction. The key parameters for controlling HS-SPME performance were optimized, including fiber coating type, temperature and absorption time settings and tea matrix modification by adding water. Quantification was carried out using matrix-matched calibration. The repeatability of measurements, expressed as relative standard deviation (R.S.D.), was less than 24% for all analytes. The limits of quantification ranged from 1 to 28 microgkg(-1). The optimized method was applied to analyze real life samples obtained from a retail market. Results generated by the new SPME procedure and those obtained by using a conventional one involving ethyl acetate extraction and high-performance gel permeation chromatography (HPGPC) clean up agreed with each other for positive (containing residue) samples.
Blood is a complex biological matrix providing valuable information on nutritional, metabolic, and immune status. The detection of blood biomarkers requires sensitive analytical methods because analytes are at very low concentrations. Peripheral blood monocytes play a crucial role in inflammatory processes, and the metabolites released by monocytes during these processes might serve as important signalling molecules and biomarkers of particular physiological states. Headspace solid-phase microextraction (HS-SPME) combined with two different mass spectrometric platforms, two-dimensional (2D) gas chromatography coupled to time-of-flight mass spectrometry (2D-GC/TOF-MS) and one-dimensional gas chromatography coupled to Orbitrap mass spectrometry (GC/Orbitrap-MS), were applied for the investigation of volatile organic compounds (VOCs) produced by human peripheral blood monocytes. An optimized method was subsequently applied for the characterization of changes in VOCs induced by lipopolysaccharides (LPS) and zymosan (ZYM) stimulation. Overall, the 2D-GC/TOF-MS and the 1D-GC/Orbitrap-MS analyses each yielded about 4000 and 400 peaks per sample, respectively. In total, 91 VOCs belonging to eight different chemical classes were identified. The samples were collected in two fractions, conditioned media for monitoring extracellularly secreted molecules and cell pellet samples to determine the intracellular composition of VOCs. Alcohols, ketones, and hydrocarbons were the main chemical classes of the metabolic profile identified in cell fractions. Aldehydes, acids and cyclic compounds were characteristic of the conditioned media fraction. Here we demonstrate that HS-SPME-2D-GC/TOF-MS is more suitable for the identification of specific VOC profiles produced by human monocytes than 1D-GC/Orbitrap-MS. We define the signature of VOCs occurring early after monocyte activation and characterise the signalling compounds released by immune cells into media.
- MeSH
- lidé MeSH
- mikroextrakce na pevné fázi MeSH
- monocyty metabolismus MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí metody MeSH
- reprodukovatelnost výsledků MeSH
- těkavé organické sloučeniny * analýza izolace a purifikace metabolismus MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
Automated head-space solid-phase microextraction (HS-SPME)-based sampling procedure, coupled to gas chromatography-time-of-flight mass spectrometry (GC-TOFMS), was developed and employed for obtaining of fingerprints (GC profiles) of beer volatiles. In total, 265 speciality beer samples were collected over a 1-year period with the aim to distinguish, based on analytical (profiling) data, (i) the beers labelled as Rochefort 8; (ii) a group consisting of Rochefort 6, 8, 10 beers; and (iii) Trappist beers. For the chemometric evaluation of the data, partial least squares discriminant analysis (PLS-DA), linear discriminant analysis (LDA), and artificial neural networks with multilayer perceptrons (ANN-MLP) were tested. The best prediction ability was obtained for the model that distinguished a group of Rochefort 6, 8, 10 beers from the rest of beers. In this case, all chemometric tools employed provided 100% correct classification. Slightly worse prediction abilities were achieved for the models "Trappist vs. non-Trappist beers" with the values of 93.9% (PLS-DA), 91.9% (LDA) and 97.0% (ANN-MLP) and "Rochefort 8 vs. the rest" with the values of 87.9% (PLS-DA) and 84.8% (LDA) and 93.9% (ANN-MLP). In addition to chromatographic profiling, also the potential of direct coupling of SPME (extraction/pre-concentration device) with high-resolution TOFMS employing a direct analysis in real time (DART) ion source has been demonstrated as a challenging profiling approach.
An efficient method combining the headspace solid-phase microextraction (HS-SPME) sampling procedure and comprehensive two-dimensional gas-chromatography/time-of-flight mass spectrometry (GC×GC/TOF-MS) was established to study the volatile secretion components of stink bugs (Heteroptera: Pentatomidae). The combined power of this approach is illustrated by the identification of fifty-seven compounds in the secretion of a European stink-bug representative, Graphosoma lineatum. (E)-4-oxohex-2-enal and (E)-dec-2-enal were found to be the major components in the adult bug secretions followed by lower amounts of n-alkenal (C₅-C₁₂), n-alkenyl acetate (C₅-C₁₁), n-alkane (C₁₁-C₁₇) homologs, dienals and other compounds. More than thirty known compounds have been identified that had not been described before in G. lineatum adults. Of these compounds, (E)-4-oxohex-2-enal is of particular interest, since its isolation and identification, while calling some previous reports into question, clearly demonstrates a potential ability of our approach to yield artifact-free secretion profiles.
- MeSH
- aldehydy analýza MeSH
- alkeny analýza MeSH
- Heteroptera chemie fyziologie MeSH
- mikroextrakce na pevné fázi metody MeSH
- odoranty analýza MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí metody MeSH
- těkavé organické sloučeniny analýza MeSH
- zvířata MeSH
- Check Tag
- mužské pohlaví MeSH
- ženské pohlaví MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
Instrumental human scent analysis is undoubtedly desirable for many forensic as well medical applications. Most of the previous human scent studies were focused on volatile organic compounds (VOCs) which were analysed by head space solid phase micro-extraction gas chromatography/mass spectrometry (HS-SPME-GC/MS). This method is, however, significantly less sensitive to "heavier" less volatile compounds emitted from the human skin. These less volatile organic scent molecules probably create the basis of the individual human scent signature, and therefore, our attention is focused mainly on these "heavier" compounds. The human scent was adsorbed onto purified glass beads and samples were prepared as hexane solutions obtained by extraction from the sampled glass beads. To resolve a lot of very similar molecules, the comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometer (GCxGC-TOFMS) was used to analyse the hexane scent solutions. Using this technique, more than 137 less volatile molecules including organic fatty acids, ketones, aldehydes, simple esters, alcohols, and especially various fatty acid esters with different carbon chains were identified. A considerable number of these molecules were identified in the scent samples for the first time.
- MeSH
- adsorpce MeSH
- lidé MeSH
- mikroextrakce na pevné fázi metody MeSH
- pleťový krém chemie MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí přístrojové vybavení metody MeSH
- těkavé organické sloučeniny chemie izolace a purifikace MeSH
- Check Tag
- lidé MeSH
- ženské pohlaví MeSH
- Publikační typ
- časopisecké články MeSH
- hodnotící studie MeSH
