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The objective of this study was to evaluate the effect of heat stress on meta-taxonomic and metabolic profiles of prokaryotes in beef cattle rumen. Six pure-breed Nellore heifers with ruminal cannulas were used in the study. Six treatments were tested in a 6 × 6 Latin Square with six periods of 21days. The treatments were evaluated in a 2 × 2 + 2 factorial arrangement, consisting of 4 combinations: two temperatures conditions (thermoneutral, TN: 24 °C; and heat stress, HS: 34 °C) and two dietary energy concentration [low-energy (37% non-fibrous carbohydrates - NFC, 12 Mcal of metabolizable energy per kg of dry matter) or high-energy concentration (50.5% NFC, 18.49 Mcal of metabolizable energy per kg of dry matter)] plus two additional treatments with animals maintained in TN conditions but with your intake restricted (TN-RI) to the same of the heifers in HS with the two dietary energy concentration. The meta-genome was sequenced by MiSeq Sequencing System platform, and the DNA sequences were analysed using Geneious 10.2.3 software. The metabolic profile was evaluated by liquid and gas chromatography. Animals under HS presented lower (P = 0.04) prokaryote richness than animals under TN conditions. The genera Flavonifractor (1.4%), Treponema (0.6%) and Ruminococcus (0.9%) showed the lowest (P < 0.04) and Carnobacterium (7.7%) the highest (P = 0.02) relative abundance when the animals were submitted to HS, in relation to animals in TN. A total of 49 different metabolites were identified in the ruminal samples. The concentration of isobutyric acid (4.32 mM) was highest in bovine rumen under HS conditions. Heat stress influenced the microbiota and concentration of some organic acids in beef cattle rumen. There was a reduction in the richness of rumen in cattle under heat stress, but the diversity of prokaryotes was not affected.
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Ácidos Carboxílicos/metabolismo , Microbiota , Rúmen/metabolismo , Rúmen/microbiologia , Animais , Bactérias/genética , Bactérias/isolamento & purificação , Bovinos , Doenças dos Bovinos/microbiologia , Feminino , Transtornos de Estresse por Calor/microbiologia , Transtornos de Estresse por Calor/veterinária , Resposta ao Choque Térmico , Umidade , Methanobrevibacter/genética , Methanobrevibacter/isolamento & purificação , RNA Ribossômico 16S/genética , TemperaturaRESUMO
Aroma profiles, key aroma compound quantification, and cluster analysis of 15 brands of extra-virgin olive oils (EVOOs) from three countries (Spain, Italy, and Greece) were investigated in the current study. Aroma compounds were isolated from the oil by using solvent-assisted flavor evaporation (SAFE) and solid-phase micro-extraction (SPME) and analyzed by gas chromatography-olfactometry mass spectrometry (GC-MS/O). A total of 89 compounds were screened by SPME/SAFE-GC-MS/O with chromatographic columns in 15 brands of samples. Eighty and 54 compounds were respectively identified by SPME- and SAFE-GC-MS/O. Of those, 44 compounds were detected by both methods. Undecanol, (Z)-4-decenal, (E)-2-dodecenal, and 2-nonanone extracted by SAFE were not found in EVOOs before. Eight classes of aroma compounds were identified, including 17 alcohols, 22 aldehydes, 9 ketones, 4 acids, 14 esters, 5 aromatics, 12 alkene, and 6 others. Eleven compounds were identified as the key aroma compounds in alternative brands of EVOOs by SAFE-aroma extract dilution analysis (AEDA). Hexanal, (E)-2-hexenal, (E)-3-hexenol, acetic acid, and (E)-2-heptenal were the common key aroma compounds by AEDA and odor activity values (OAVs). From the cluster analysis of the heatmap, the aroma compounds of all the Spain EVOOs were similar, and there were some differences from the samples of Italy and Greece. It suggested that both the amount and concentration of aroma compounds determine the similarity of aroma in EVOOs.
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Azeite de Oliva/análise , Compostos Orgânicos Voláteis/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Olfatometria/métodos , Microextração em Fase Sólida/métodos , Compostos Orgânicos Voláteis/químicaRESUMO
The aims of this study were to evaluate the bioavailability of polycyclic aromatic hydrocarbons (PAHs) in industrial and agricultural soils using chemical methods and a bioassay, and to study the relationships between the methods. This was conducted by comparing the quantities of PAHs extracted from two manufactured gas plant (MGP) soils and an agricultural soil with low level contamination by solid-phase micro-extraction (SPME) and Tenax-TA extraction with the quantities taken up by the earthworm (Eisenia fetida). In addition, a biodegradation experiment was conducted on one MGP soil (MGP-A) to clarify the relationship between PAH removal by biodegradation and the variation in PAH concentrations in soil pore water. Results demonstrated that the earthworm bioassay could not be used to examine PAH bioavailability in the tested MGP soils; which was the case even in the diluted MGP-A soils after biodegradation. However, the bioassay was successfully applied to the agricultural soil. These results suggest that earthworms can only be used for bioassays in soils with low toxicity. In general, rapidly desorbing concentrations extracted by Tenax-TA could predict PAH concentrations accumulated in earthworms (R2=0.66), while SPME underestimated earthworm concentrations by a factor of 2.5. Both SPME and Tenax extraction can provide a useful tool to predict PAH bioavailability for earthworms, but Tenax-TA extraction was proven to be a more sensitive and precise method than SPME for the prediction of earthworm exposure in the agricultural soil.
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Oligoquetos/metabolismo , Hidrocarbonetos Policíclicos Aromáticos/farmacocinética , Solo/química , Agricultura , Animais , Biodegradação Ambiental , Bioensaio/métodos , Disponibilidade Biológica , Gases , Indústrias , Hidrocarbonetos Policíclicos Aromáticos/toxicidade , Polímeros/farmacocinética , Poluentes do Solo/farmacocinética , Poluentes do Solo/toxicidade , Extração em Fase Sólida/métodosRESUMO
The five studied bacterial strains could produce volatile organic compounds (VOCs) that kill nematodes. Based on their 16S rRNA sequences, these strains were identified as Pseudochrobactrum saccharolyticum, Wautersiella falsenii, Proteus hauseri, Arthrobacter nicotianae, and Achromobacter xylosoxidans. The bacterial VOCs were extracted using solid-phase micro-extraction (SPME) and subsequently identified by GC/MS analysis. The VOCs covered a wide range of aldehydes, ketones, alkyls, alcohols, alkenes, esters, alkynes, acids, ethers, as well as heterocyclic and phenolic compounds. Among the 53 VOCs identified, 19 candidates, produced by different bacteria, were selected to test their nematicidal activity (NA) against Caenorhabditis elegans and Meloidogyne incognita. The seven compounds with the highest NAs were acetophenone, S-methyl thiobutyrate, dimethyl disulfide, ethyl 3,3-dimethylacrylate, nonan-2-one, 1-methoxy-4-methylbenzene, and butyl isovalerate. Among them, S-methyl thiobutyrate showed a stronger NA than the commercial insecticide dimethyl disulfide. It was reported for the first time here that the five bacterial strains as well as S-methyl thiobutyrate, ethyl 3,3-dimethylacrylate, 1-methoxy-4-methylbenzene, and butyl isovalerate possess NA. These strains and compounds might provide new insights in the search for novel nematicides.
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Bactérias/química , Nematoides/efeitos dos fármacos , Controle de Pragas , Plantas/parasitologia , Compostos Orgânicos Voláteis/química , Compostos Orgânicos Voláteis/toxicidade , Animais , Caenorhabditis elegans/efeitos dos fármacos , Cromatografia Gasosa-Espectrometria de Massas , Controle de Pragas/métodos , Microextração em Fase Sólida , Compostos Orgânicos Voláteis/isolamento & purificaçãoRESUMO
The presented study investigates the use of passive sampling, i.e. solid phase microextraction with polydimethylsiloxane fibers (PDMS-SPME), to assess the bioavailability of fiver neutral organic chemicals (phenanthrene, pyrene, lindane, p,p'-DDT, and PCB 153) spiked to natural and artificial soils after different aging times. Contaminant bioavailability was assessed by comparing PDMS concentrations with results from a 10 day bioaccumulation test with earthworms (Eisenia fetida). The hypotheses tested were (i) organic carbon (OC) normalization, which is commonly used to account for sorption and bioavailability of hydrophobic organic chemicals in soil risk assessment, has limitations due to differences in sorptive properties of OC and aging processes (i.e. sequestration and biodegradation) and (ii) PDMS-SPME provides a more reliable measure of soil contaminant bioavailability than OC normalized soil concentrations. The above stated hypotheses were confirmed since the results showed that: (i) the PDMS/soil organic carbon partition ratio (R) accounting for the role that OC plays in partitioning significantly differed between soils and aging times and (ii) the correlation with earthworm concentrations was better using porewater concentrations derived from PDMS concentrations than when organic normalized soil concentrations were used. Capsule: Sorption of organic compounds measured by SPME method and their bioavailability to earthworms cannot be reliably predicted using OC content.
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Oligoquetos/química , Oligoquetos/metabolismo , Poluentes do Solo/química , Poluentes do Solo/metabolismo , Microextração em Fase Sólida , Animais , Monitoramento Ambiental , Compostos Orgânicos/análise , Compostos Orgânicos/metabolismoRESUMO
Common bunt disease of wheat in China is caused mainly by Tilletia foetida. However, reliable approaches for determining disease-associated biochemical markers are rarely reported. Here, a headspace-solid-phase microextraction coupled with headspace GC-tandem mass spectrometry (HS-SPME-GC-MS) was used to screen volatile substances in infected wheat, and an optimal chemical marker was selected to establish analytical methods for disease determination. Non-targeted screening of 13 volatile compounds unique to diseased wheat allowed a metabolite with rotten fish-like smell, trimethylamine (TMA), to be selected as the inspection marker. Subsequently, two analytical methodologies, HS-SPME-GC-MS and headspace gas chromatography with flame ionization detection (HS-GC-FID), were established to determinate the TMA content in wheat. The linear relationship, recovery and reproducibility of the methods were validated. The limit of detection (LOD) was 0.02 µg/kg for the former method, 5000-fold lower than that for the latter. When analysing samples, HS-SPME-GC-MS showed excellent sensitivity and allowed for the determination of 0.05% infected kernels among whole wheat grains. Therefore, TMA determination using HS-SPME-GC-MS is an effective alternative method to detect wheat common bunt disease occurring at extremely low infection rate.
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Microextração em Fase Sólida , Compostos Orgânicos Voláteis , Animais , Microextração em Fase Sólida/métodos , Triticum , Cromatografia Gasosa-Espectrometria de Massas/métodos , Reprodutibilidade dos Testes , Compostos Orgânicos Voláteis/análiseRESUMO
Locating underground pipeline leaks can be challenging due to their hidden nature and variable terrain conditions. To sample soil gas, solid-phase microextraction (SPME) was employed, and a portable gas chromatography/mass spectrometry (GC/MS) was used to detect the presence and concentrations of petroleum hydrocarbon volatile organic compounds (pH-VOCs), including benzene, toluene, ethylbenzene, and xylene (BTEX). We optimized the extraction method through benchtop studies using SPME. The appropriate fibre materials and exposure time were selected for each BTEX compound. Before applying SPME, we preconditioned the soil vapour samples by keeping the temperature at around 4 °C and using ethanol as a desorbing agent and moisture filters to minimize the impact of moisture. To conduct this optimisation, airbags were applied to condition the soil vapour samples and SPME sampling. By conditioning the samples using this method, we were able to improve analytical efficiency and accuracy while minimizing environmental impacts, resulting in more reliable research data in the field. The study employed portable GC/MS data to assess the concentration distribution of BTEX in soil vapour samples obtained from 1.5 m below the ground surface at 10 subsurface vapour monitoring locations at the leak site. After optimization, the detection limits of BTEX were almost 100 µg/m3, and the measurement repeatabilities were approximately 5% and 15% for BTEX standards in the laboratory and soil vapour samples in the field, respectively. The soil vapour samples showed a hotspot region with high BTEX concentrations, reaching 30 mg/m3, indicating a diesel return pipeline leak caused by a gasket failure in a flange. The prompt detection of the leak source was critical in minimizing environmental impact and worker safety hazards.
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Petróleo , Microextração em Fase Sólida , Cromatografia Gasosa-Espectrometria de Massas/métodos , Microextração em Fase Sólida/métodos , Petróleo/análise , Derivados de Benzeno/análise , Tolueno/análise , Benzeno/análise , Xilenos/análise , Solo , Medição de RiscoRESUMO
Tea (Camellia sinensis) is one of the most popular beverages worldwide. Many types of tea products continuously emerge in an endless stream; so, the classification of tea becomes more difficult. Aroma is a vital indicator of tea quality. The present study deals with the identification of aroma compounds in 18 different kinds of tea belonging to three typical tea varieties, including green tea, oolong tea, and black tea, using GC-IMS and GC × GC-O-MS. Moreover, the clustering of all 18 tea samples and the in depth correlation analysis between sensory evaluation and instrumental data were performed using the PCA and OPLS-DA. The results revealed that in all 18 kinds of tea, a total of 85 aroma compounds were detected by GC-IMS, whereas 318 were detected by GC × GC-O-MS. The PCA result revealed that green tea, oolong tea, and black tea could be clearly separated based on their peak areas. The OPLS-DA result showed that a total of 49 aroma compounds with VIP value > 1.0 could be considered as the potential indicators to quickly classify or verify tea types. This study not only compared the aroma differences across different types of teas, but also provided ideas for the rapid monitoring of tea quality and variety.
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The goal of this study was to assess nutrient primary metabolites and aroma determinants in Prunus armeniaca L. fruits and seed kernels grown in Egypt represented by its different cultivars and agricultural conditions i.e., two different soil types (muddy versus sandy). Two techniques were employed to assess non-volatile and volatile metabolites using gas chromatography mass-spectrometry (GC-MS) post silylation, and headspace solid-phase micro-extraction (HS-SPME) coupled GC-MS, respectively. A total of 36 peaks belonging to sugars, fatty acids/esters and organic acids were identified by GC-MS in various apricot fruits and seed kernels cultivars. Glucose and sucrose were enriched in apricot fruits compared to the seed kernels. A total of 70 volatiles were identified, with lactones, alcohols and esters representing the main classes of apricot volatiles accounting for its discrete aroma. (E)-Anethole, ß-ionone, γ-decanolactone and methyl palmitate were the major peaks contributing to the discrimination between various fruit cultivars and providing novel insight on apricot metabolome.
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The compounds in volatile flavor substances in duck meats of three different body parts (breast, leg, and wing) were extracted by headspace solid-phase micro-extraction and determined by gas chromatography-mass spectrometry. A total of 16 main volatile compounds including 4 hydrocarbons, 4 alcohols, 2 acids, 3 aldehydes, and 3 others (N-containing, S-containing) were identified in raw duck meats from three different body parts. The hydrocarbon compounds account for more than 50% of all volatile substances in all three body parts. And the percentage of hydrocarbon compounds in raw duck breast meat reaches 82.76%. A total of 81 volatile compounds including 15 hydrocarbons, 10 alcohols, 7 acids, 12 aldehydes, 4 esters, 19 S-containing and N-containing compounds, and 14 others were isolated and identified in 1 hr-marinated and cooked duck meats. A total of 101 kinds of volatile flavor compounds including 13 hydrocarbons, 14 alcohol, 7 acids, 8 aldehydes, 12 esters, 23 S-containing and N-containing compounds, and 24 others were detected in 3 hr-marinated duck meats of the three body parts. It was proved in this study that under the same conditions, the volatile compounds in duck legs are more than those in duck breasts and wings, and the types of volatile flavor substances increase significantly in duck meats after cooked. PRACTICAL APPLICATIONS: Prepared and cooked duck meat, especially wings and legs are popular food in China. The results suggest that Pickling makes duck meat more flavory while proper pickling time is less than 3 hr. Duck wings are better for marinating and cooking compared with duck breasts and legs. The acceptance study of duck meat from different body parts and the analysis of volatile flavor compounds are beneficial for optimizing utilization of whole parts of duck meat.
Assuntos
Compostos Orgânicos Voláteis , Álcoois/análise , Aldeídos , Animais , Patos , Ésteres , Carne/análise , Compostos Orgânicos Voláteis/químicaRESUMO
In this review, we summarize the methods of sample introduction into a gas chromatograph. For volatile organic compounds, headspace measurements and purge-trap methods have been used traditionally. Recently, the trapped headspace method has been used in water quality testing. In addition, various solid-state adsorption methods have been developed, including a method in which the adsorbent is placed inside a needle, while new adsorbents and their applications have also been introduced.
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BACKGROUND: Different organisms such as bacteria, molds and humans produce and release a relative unknown class of metabolites which are responsible for the individual olfactory pattern. These volatile organic metabolites (VOM) represent a kind of biosignature that reflects the sum of all multifactorial influences, including genetics, environmental factors, nutritional and disease status. As a result of pathological processes the individual body odor can be influenced by newly produced or altered compositions of the VOM. Until now, human VOM have been detected in various body media, such as on the skin, in the exhaled air as well as in body fluids such as saliva, mother's milk, sweat, blood and urine. METHODS: In this retrospective case-control study urinary VOM of 53 therapy-naive patients with head and neck squamous cell carcinoma (HNSCC) and 82 healthy controls were semi-quantified by headspace solid-phase micro extraction (SPME) gas chromatography (GC) mass spectrometry (MS). At first, the procedure was optimized in respect to the extraction parameters. By using Student's t-test significant differences in the VOM pattern with the corresponding p-values were obtained. For multivariate metabolite pattern recognition the hierarchical cluster analysis by Ward was applied, followed by the supervised partial least squares-discriminant analysis (PLS-DA). RESULTS: In total 81 VOMs could identified in the urine samples of all study participants, of which 25 were significantly increased and of which were 10 significantly reduced in HNSCC-patients compared to the controls. In addition, the multivariate statistics confirmed that on the basis of the renal excreted pattern of the volatile metabolites a high discrimination can be carried out between patients with a tumor in the head and neck region and controls. The substance group of the saturated, unbranched aldehydes makes a substantial contribution in this context. CONCLUSIONS: The systematic pattern analysis of urinary VOMs appears to have potential clinical application as a diagnostic tool for cancer, especially HNSCC.
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Biomarcadores Tumorais/urina , Carcinoma de Células Escamosas/urina , Neoplasias de Cabeça e Pescoço/urina , Compostos Orgânicos Voláteis/urina , Estudos de Casos e Controles , Feminino , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Masculino , Análise Multivariada , Estudos Retrospectivos , Microextração em Fase Sólida , Compostos Orgânicos Voláteis/metabolismoRESUMO
Microfluidic chips coupling with mass spectrometry (MS) will be of great significance to the development of relevant instruments involving chemical and bio-chemical analysis, drug detection, food and environmental applications and so on. In our previous works, we proposed two types of microfluidic electrospray ionization (ESI) chip coupling with MS: the two-phase flow focusing (FF) ESI microfluidic chip and the corner-integrated ESI emitter, respectively. However the pretreatment module integrated with these ESI emitters is still a challenging problem. In this paper, we concentrated on integrating the solid phase micro-extraction (SPME) module with our previous proposed on-chip ESI emitters; the fabrication processes of such SPME module are fully compatible with our previous proposed ESI emitters based on the multi-layer soft lithography. We optimized the structure of the integrated chip and characterized its performance using standard samples. Furthermore, we verified its abilities of salt removal, extraction of multiple analytes and separation through on-chip elution using mimic biological urine spiked with different drugs. The results indicated that our proposed integrated module with ESI emitters is practical and effective for real biological sample pretreatment and MS detection.
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Human scent has been demonstrated to allow for the differentiation of individuals. The extent of this differentiation may allow scent to be used as a characteristic, capable of revealing information on an individual's traits. The ability to use scent as a biometric human feature has enabled the use of scent as forensic evidence. However, its reliability, value, and admissibility in courts of law have sometimes been challenged as a result of limited scientific validation. Full acceptance of human scent evidence has been hindered by the limited availability of peer reviewed information that provides greater understanding of how human scent originates and how it may be used. The objective of this study is to report new data that further enhances our understanding of the value of human scent evidence and its acceptance in courts of law. In order to fulfill this objective, volatile organic compound combinations were identified as markers for race/ethnicity and gender from hand odor samples from 105 individuals. The accuracy of human classification by race/ethnicity and gender, on the basis of these markers, was determined and validated. Overall accuracies of 80% and 72% were obtained for the classification of subjects by gender and race/ethnicity, respectively. The results obtained demonstrate that the identified VOC marker combinations represent a viable resource for the classification and/or differentiation of persons of interest and, as such, may be considered a valuable forensic tool for subject identification.
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Odorantes/análise , Compostos Orgânicos Voláteis/análise , Adolescente , Adulto , Idoso , Biomarcadores/análise , Feminino , Cromatografia Gasosa-Espectrometria de Massas , Mãos , Humanos , Masculino , Pessoa de Meia-Idade , Grupos Raciais , Reprodutibilidade dos Testes , Fatores Sexuais , Microextração em Fase Sólida , Adulto JovemRESUMO
The aim of this study was to demonstrate the variations in bioavailability remaining in industrial and agricultural soils contaminated by polycyclic aromatic hydrocarbons (PAHs) after bioremediation. After inoculation of Mycobacterium sp. and Mucor sp., PAH biodegradation was tested on a manufactured gas plant (MGP) soil and an agricultural soil. PAH bioavailability was assessed before and after biodegradation using solid-phase extraction (Tenax-TA extraction) and solid-phase micro-extraction (SPME) to represent bioaccessibility and chemical activity of PAHs, respectively. Only 3- and 4-ring PAHs were noticeably biodegradable in the MGP soil. PAH biodegradation in the agricultural soil was different from that in the MGP soil. The rapidly desorbing fractions (F(rap)) extracted by Tenax-TA and the freely dissolved concentrations of 3- and 4-ring PAHs determined by SPME from the MGP soil decreased after 30 days biodegradation; those values of the 5- and 6-ring PAHs changed to a lesser degree. For the agricultural soil, the F(rap) values of the 3- and 4-ring PAHs also decreased after the biodegradation experiment. The Tenax-TA extraction and the SPME have the potential to assess variations in the bioavailability of PAHs and the degree of biodegradation in contaminated MGP soils. In addition, Tenax-TA extraction is more sensitive than SPME when used in the agricultural soil.
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Hidrocarbonetos Policíclicos Aromáticos/metabolismo , Poluentes do Solo/metabolismo , Agricultura , Biodegradação Ambiental , Disponibilidade Biológica , Mucor/metabolismo , Mycobacterium/metabolismo , Indústria de Petróleo e Gás , Hidrocarbonetos Policíclicos Aromáticos/química , Polímeros/química , Solo , Microbiologia do Solo , Poluentes do Solo/química , Extração em Fase SólidaRESUMO
This article reports on the chemical analysis of molecular profiles of tarsal secretions of the desert locust Schistocerca gregaria (Forsskål, 1775) by gas chromatography hyphenated with quadrupol mass spectrometry (GC-MS) as well as (1)H-nuclear magnetic resonance ((1)H NMR) spectroscopy. Special focus of this study was to elaborate on sampling methods which enable selective microscale extraction of insect secretions in a spatially controlled manner, in particular tarsal adhesive secretions and secretions located on cuticle surfaces at the tibia. Various solvent sampling procedures and contact solid-phase microextraction (SPME) methods were compared in terms of comprehensiveness and extraction efficiencies as measured by signal intensities in GC-MS. Solvent sampling with water as extraction solvent gave access to the elucidation of chemical profiles of polar compound classes such as amino acids and carbohydrates, but is extremely tedious. Contact SPME on the other hand can be regarded as a simplified and more elegant alternative, in particular for the lipophilic compound fraction. Many proteinogenic amino acids and ornithine as well as carbohydrate monomers arabinose, xylose, glucose, and galactose were detected in tarsal secretions after acid hydrolysis of aqueous extracts. Qualitatively similar but quantitatively significantly different molecular profiles were found for the lipid fraction which contained mainly n-alkanes and internally branched monomethyl-, dimethyl-, and trimethyl-alkanes in the C23-C49 range as well as long chain fatty acids and aldehydes. Especially, hydrocarbons with >C40 carbon numbers have previously been rarely reported for insect secretions. The results suggest that the investigated insect secretions are complex emulsions which allow the attachment of tarsi on various otherwise incompatible materials of smooth and rough surfaces. The solid consistence of the established alkanes at ambient temperatures might contribute to a semi-solid consistence of the adhesive, amalgamating partly opposing functions such as slip resistance, tarsal release, desiccation resistance, and mechanical compliance. The methods developed can be extended to other similar applications of studying compositions of insect secretions of other species.
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Cromatografia Gasosa-Espectrometria de Massas/métodos , Gafanhotos/metabolismo , Animais , Microextração em Fase SólidaRESUMO
Analysis of headspace concentrations of diphenylamine using solid phase micro-extraction (SPME) was examined for its suitability to detect DPA contamination and off-gassing in apple (Malus domestica) fruit, storage rooms and storage materials. Four SPME fibre coatings including polydimethylsiloxane (PDMS, 100 µm), PDMS/divinylbenzene (PDMS/DVB), Polyacrylate (PA) and PDMS 7 µm were evaluated. The average limits of detection and of quantification for head space DPA ranged from 0.13 to 0.72 µg L(-1) and 0.42 to 2.35 µg L(-1), respectively. Polyacrylate was identified to be the most suitable and compatible fibre for DPA analysis in apple samples, because of its high sensitivity to DPA and low fruit volatile interferences. SPME techniques were further applied to study contamination of DPA in apples, storage rooms and packaging materials. DPA was found in the air of storage rooms containing apples that were not treated with DPA. Wood and plastic bin material, bin liners, and foam insulation all adsorbed and off-gassed DPA and could be potential sources of contamination of untreated apples.
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Difenilamina/química , Frutas/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Malus/química , Microextração em Fase Sólida/métodos , Aditivos Alimentares/análise , Armazenamento de AlimentosRESUMO
The characteristics of an individual's odor from sweat, breath and skin provide important information for criminal tracking in field of forensic science. Solid phase micro-extraction gas chromatography/mass spectrometry (SPME-GC/MS) was used to determine human sweat volatile organic compounds (VOCs) profiles. The mass spectrometric analysis (with electron impact mode) followed by 2nd dimensional separation with two different GC columns (one polar and one relatively nonpolar) connected in parallel were used to identify the 574 compounds from sweat samples. The components included alcohols, aldehydes, aliphatics/aromatics, carboxylic acids, esters, ketones, and other organic compounds (amides/amines, thio/thioesters, oxide, sulfides, nitro compounds). Of these compounds, 1-tridecanol, 1,3-bis(1,1-dimethyl ethyl)-benzene, 4,4'-(1-methylethylidene) bis-phenol and 7-acetyl-6-ethyl-1,1,4,4,-tetramethyl-tetraline were common components in all donor's sweat volatile samples. Age-related specific compounds were also detected. The results suggest that characteristic volatile profiles of human sweat emanations could provide the valuable information to forensic scientists.
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Odorantes/análise , Suor/química , Compostos Orgânicos Voláteis/análise , Adulto , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Masculino , Pessoa de Meia-Idade , República da CoreiaRESUMO
Cucumis melo fruit is highly valued for its sweet and refreshing flesh, however the flavour and value are also highly influenced by aroma as dictated by volatile organic compounds (VOCs). A simple and robust method of sampling VOCs on polydimethylsiloxane (PDMS) has been developed. Contrasting cultivars of C. melo subspecies melo were investigated at commercial maturity: three cultivars of var. Cantalupensis group Charentais (cv. Cézanne, Escrito, and Dalton) known to exhibit differences in ripening behaviour and shelf-life, as well as one cultivar of var. Cantalupensis group Ha'Ogan (cv. Noy Yisre'el) and one non-climacteric cultivar of var. Inodorus (cv. Tam Dew). The melon cultivar selection was based upon fruits exhibiting clear differences (cv. Noy Yisre'el and Tam Dew) and similarities (cv. Cézanne, Escrito, and Dalton) in flavour. In total, 58 VOCs were detected by thermal desorption (TD)-GC-MS which permitted the discrimination of each cultivar via Principal component analysis (PCA). PCA indicated a reduction in VOCs in the non-climacteric cv. Tam Dew compared to the four Cantalupensis cultivars. Within the group Charentais melons, the differences between the short, mid and long shelf-life cultivars were considerable. ¹H NMR analysis led to the quantification of 12 core amino acids, their levels were 3-10-fold greater in the Charentais melons, although they were reduced in the highly fragrant cv. Cézanne, indicating their role as VOC precursors. This study along with comparisons to more traditional labour intensive solid phase micro-extraction (SPME) GC-MS VOC profiling data has indicated that the high-throughput PDMS method is of great potential for the assessment of melon aroma and quality.
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Cucumis melo/metabolismo , Frutas/metabolismo , Metabolômica , Odorantes/análise , Compostos Orgânicos Voláteis/análise , Cucumis melo/química , Frutas/química , Compostos Orgânicos Voláteis/metabolismoRESUMO
Fifty years after the term "pheromone" was coined by Peter Karlson and Martin Lüsher the search for these semiochemicals is still an elusive goal of chemical ecology and communication studies. Contrary to what appears in the popular press, the race is still on to capture and define human scents. Over the last several years, it became increasingly clear that pheromone-like chemical signals probably play a role in offspring identification and mother recognition. Recently, we analyzed the volatile compounds in sweat patch samples collected from the para-axillary and nipple-areola regions of women during pregnancy and after childbirth. We hypothesized that, at the time of birth and during the first weeks of life, the distinctive olfactory pattern of the para-axillary area is probably useful to newborns for recognizing and distinguishing their own mother, whereas the characteristic pattern of the nipple-areola region is probably useful as a guide to nourishment.