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Gas Chromatography-mass Spectrometry (gas + chromatography-mass_spectrometry)
Terms modified by Gas Chromatography-mass Spectrometry Selected AbstractsThe importance of scent and nectar filters in a specialized wasp-pollination systemFUNCTIONAL ECOLOGY, Issue 5 2009Adam Shuttleworth Summary 1.,Plants with open flowers and exposed nectar should attract a wide diversity of flower visitors, yet, for reasons that are not yet well understood, some plants with these ,generalist' floral traits have highly specialized pollination systems. 2.,We investigated this problem in the African milkweed Pachycarpus grandiflorus which has open flowers that produce copious amounts of exposed and concentrated nectar, yet is visited almost exclusively by spider-hunting wasps in the genus Hemipepsis. 3.,These wasps were the only visitors found to consistently carry pollinaria and a cage experiment showed that they are capable of successfully pollinating this plant. Furthermore, experimental hand-pollinations showed that P. grandiflorus is genetically self-incompatible and thus reliant on pollinators for seed set. 4.,We investigated the roles of chemical (nectar and floral scent) and spectral properties in the selective attraction of wasps and the filtering out of other potential flower visitors. Nectar palatability experiments showed that the nectar is unpalatable to honeybees but palatable to the wasps. Choice experiments conducted in the field and using a Y-maze in the laboratory showed that wasps are attracted primarily by scent rather than visual cues. Analysis of scent using Gas Chromatography-Mass Spectrometry showed that these inflorescences produce 36 different compounds, mostly monoterpenes and aliphatics. Analysis of spectral reflectance showed that flowers have similar colouring to the background vegetation. 5.,We conclude that P. grandiflorus is specialized for pollination by Hemipepsis wasps, and in the absence of morphological filters, achieves specialization through unpalatable nectar, cryptic colouring and scent as a selective pollinator attractant. 6.,This study demonstrates that plants whose flowers are not morphologically adapted to exclude particular floral visitors can achieve specialization through non-morphological filters. [source] Volatile composition and proteolysis in traditionally produced mature Kashar cheeseINTERNATIONAL JOURNAL OF FOOD SCIENCE & TECHNOLOGY, Issue 7 2009Ali Adnan Hayaloglu Summary Twelve samples of raw milk mature Kashar cheese at different stages of ripening were collected from retail outlets. The average pH, moisture, fat-in-dry matter, protein, salt-in-dry matter and titratable acidity contents of the samples were 5.33, 39.39%, 45.20%, 27.33%, 6.62% and 0.65% (as lactic acid), respectively. Indices of proteolysis varied from 10.72% to 23.75% and 7.09% to 12.26% for pH 4.6-soluble and 12% trichloroacetic acid-soluble nitrogen fractions, respectively, and total free amino acid concentrations ranged from 6.36 to 36.03 mg Leu g,1 of cheese. The cheeses were analysed for volatile compounds by Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry (GC-MS). A total of 113 compounds were detected and identified belonging to the following chemical groups: acids (eleven), esters (sixteen), ketones (sixteen), aldehydes (six), alcohols (twenty-seven), sulphur compounds (seven), terpenes (seven) and miscellaneous compounds (twenty-three). The potential effect of each compound on the flavour profile of Kashar cheese is discussed. Acids, esters, ketones and alcohols were found at considerable levels in the samples. Kashar cheeses obtained from different retail outlets displayed some differences in terms of chemical composition, proteolysis and patterns of aroma compounds; and may be attributed to their production technologies and age-related variations. [source] An automated method for peak detection and matching in large gas chromatography-mass spectrometry data setsJOURNAL OF CHEMOMETRICS, Issue 8-10 2006Sarah J. Dixon Abstract A new approach for peak detection and matching has been developed and applied to two data sets. The first consisted of the Gas Chromatography-Mass Spectrometry (GC-MS) samples of 965 human sweat samples obtained from a population of 197 individuals. The second data set contained 500 synthetic chromatograms, and was generated to validate the peak detection and matching methods. The size of both of the data sets (around 500,000 detectable peaks over all chromatograms in data set 1, and around 100,000 in data set 2) would make it unfeasible to check manually whether peaks are matched. In the method described, the first procedure involves pre-processing the data before carrying out the second procedure of peak detection. The final procedure of peak matching consists of three stages: (a) finding potential target peaks in the full data set over all chromatograms; (b) matching peaks in the chromatograms to these targets to form clusters of spectra associated with each target; (c) merging targets where appropriate. Peak detection and matching were applied to both data sets, and the importance of stage (c) of peak matching described. In addition to the analysis of the synthetic chromatograms, the method was also validated by shuffling the original order of the sweat chromatograms and performing the methods independently on the newly shuffled data. Copyright © 2007 John Wiley & Sons, Ltd. [source] ALKALOID COMPOSITION OF LUPINUS CAMPESTRIS FROM MEXICOJOURNAL OF FOOD BIOCHEMISTRY, Issue 2 2001J. MARTÍNEZ-HERRERA ABSTRACT The content of quinolizidine alkaloids (QA) in Lupinus campestris, Fabaceae family, was analyzed by Gas Chromatography-Mass Spectrometry (GC-MS), Samples of various organs of Lupinus campestris collected at different monthly stages of the growing plant, were subjected to extraction in a Merck Extrelut column. The quinolizidine alkaloid patterns of stems, leaves, flowers, pods and seeds were assessed and then identified and quantified by GC. Alkaloid structures were identified according to their mass fragmentation patterns, in combination with their indicative Kovats retention index. Alkaloids found in several developmental stages of the plant were mainly: aphyllidine, 5, 6-dehydrolupanine, aphylline, dehydro-oxosparteine, lupanine, ,-isolupanine, hydroxyaphylline and hydroxyaphyllidine, plus two alkaloids that -were not identified. During the third month the relative abundance of total alkaloids were highest. The main alkaloids found in seeds were hydroxyaphylline and hydroxyaphyllidine. [source] Age and space distributions of monoterpenes in fresh needles of Picea abies (L) Karst. determined by gas chromatography-mass spectrometryPHYTOCHEMICAL ANALYSIS, Issue 4 2001V. Holubová Abstract Monoterpenes (,- and ,-pinene, ,-3-carene, camphene, ,-phellandrene and limonene) were determined by Gas Chromatography-Mass Spectrometry in fresh needles of Picea abies (L) Karst. situated in three ecologically different regions of Moravia. Through the use of cryogenic grinding for critical sample homogenisation, solvent extraction with cold n -hexane, followed by GC analysis with mass detection, very low quantities of sample (0.1,0.3,g needles) could be processed, thus permitting a comparison of amounts of monoterpenes in needles of different ages and a determination of changes in concentrations of monoterpenes in needles at different locations on the tree. The amount of ,-phellandrene decreased with the age of the needles, and the content of ,-3-carene was higher in apical branches compared to lateral ones. Copyright © 2001 John Wiley & Sons, Ltd. [source] Performance Evaluation of the Scent Transfer UnitÔ (STU-100) for Organic Compound Collection and ReleaseJOURNAL OF FORENSIC SCIENCES, Issue 4 2006Brian A. Eckenrode Ph.D. ABSTRACT: The Scent Transfer UnitÔ (STU-100) is a portable vacuum that uses airflow through a sterile gauze pad to capture a volatiles profile over evidentiary items for subsequent canine presentation to assist law enforcement personnel. This device was evaluated to determine its ability to trap and release organic compounds at ambient temperature under controlled laboratory conditions. Gas chromatography-mass spectrometry (GC-MS) analyses using a five-component volatiles mixture in methanol injected directly into a capture pad indicated that compound release could be detected initially and 3 days after the time of collection. Additionally, 15 compounds of a 39-component toxic organic gaseous mixture (10,1000 parts per billion by volume [p.p.b.v]) were trapped, released, and detected in the headspace of a volatiles capture pad after being exposed to this mixture using the STU-100 with analysis via GC-MS. Component release efficiencies at ambient temperature varied with the analyte; however, typical values of c. 10% were obtained. Desorption at elevated temperatures of reported human odor/scent chemicals and colognes trapped by the STU-100 pads was measured and indicated that the STU-100 has a significant trapping efficiency at ambient temperature. Multivariate statistical analysis of subsequent mass spectral patterns was also performed. [source] Reactivity of C4-indolyl substituted 1,4-dihydropyridines toward superoxide anion (O2,) in dimethylsulfoxideJOURNAL OF PHYSICAL ORGANIC CHEMISTRY, Issue 6 2009Ricardo Salazar Abstract Reactivity of two new C4-indolyl substituted 1,4-dihydropyridines (1,4-DHPs) toward superoxide anion (O2,) in dimethylsulfoxide (DMSO) is reported. Reactivity was followed by electrochemical and spectroscopic techniques. Gas chromatography-mass spectrometry (GC,MS) was used to identify the final products of the reaction. C4 indolyl-substituted-1,4-DHPs reacted toward O2, at significant rates, according to the calculated kinetic rate constants. Results are compared with 4-phenyl-DHP and the commercial 1,4-DHPs, nimodipine, nisoldipine, and amlodipine. Indolyl-substituted 1,4-DHPs were more reactive than the commercial derivatives. The direct participation of proton of the 1-position of the secondary amine in the quenching of O2, was demonstrated. Copyright © 2008 John Wiley & Sons, Ltd. [source] Acute confusional state after designer tryptamine abusePSYCHIATRY AND CLINICAL NEUROSCIENCES, Issue 2 2007MASANARI ITOKAWA md Abstract A 23-year-old Japanese woman was brought to the emergency department about 6.5 h after taking liquid and later a half tablet purchased on the street. About 4.5 h prior to presentation, she displayed excited and disorganized behavior. On examination, she was not alert or oriented, with a Glasgow Coma Scale score of 13, did not answer any questions from doctors while smirking and looking around restlessly, and sometimes exhibited echolalia, imitating the speech of doctors. She was given intravenous infusion of fluid for 8 h, then discharged. Gas chromatography-mass spectrometry of urine revealed 5-methoxy-diisopropyltryptamine, 5-methoxy-N-methyltryptamine and an unidentified tryptamine. Identifying chemical products based solely on information of users is insufficient, and urinalysis is necessary in cases potentially involving designer drugs. [source] Do ,9 -tetrahydrocannabinol concentrations indicate recent use in chronic cannabis users?ADDICTION, Issue 12 2009Erin L. Karschner ABSTRACT Aims To quantify blood ,9 -tetrahydrocannabinol (THC) concentrations in chronic cannabis users over 7 days of continuous monitored abstinence. Participants Twenty-five frequent, long-term cannabis users resided on a secure clinical research unit at the US National Institute on Drug Abuse under continuous medical surveillance to prevent cannabis self-administration. Measurements Whole blood cannabinoid concentrations were determined by two-dimensional gas chromatography-mass spectrometry. Findings Nine chronic users (36%) had no measurable THC during 7 days of cannabis abstinence; 16 had at least one positive THC ,0.25 ng/ml, but not necessarily on the first day. On day 7, 6 full days after entering the unit, six participants still displayed detectable THC concentrations [mean ± standard deviation (SD), 0.3 ± 0.7 ng/ml] and all 25 had measurable carboxy-metabolite (6.2 ± 8.8 ng/ml). The highest observed THC concentrations on admission (day 1) and day 7 were 7.0 and 3.0 ng/ml, respectively. Interestingly, five participants, all female, had THC-positive whole blood specimens over all 7 days. Body mass index did not correlate with time until the last THC-positive specimen (n = 16; r = ,0.2; P = 0.445). Conclusions Substantial whole blood THC concentrations persist multiple days after drug discontinuation in heavy chronic cannabis users. It is currently unknown whether neurocognitive impairment occurs with low blood THC concentrations, and whether return to normal performance, as documented previously following extended cannabis abstinence, is accompanied by the removal of residual THC in brain. These findings also may impact on the implementation of per se limits in driving under the influence of drugs legislation. [source] On-line identification of lysergic acid diethylamide (LSD) in tablets using a combination of a sweeping technique and micellar electrokinetic chromatography/77 K fluorescence spectroscopyELECTROPHORESIS, Issue 6 2003Ching Fang Abstract This work describes a novel method for the accurate determination of lysergic acid diethylamide (LSD) in tablets. A technique involving sweeping-micellar electrokinetic chromatography (MEKC) was used for the initial on-line concentration and separation, after which a cryogenic molecular fluorescence experiment was performed at 77 K. Using this approach, not only the separation of LSD from the tablet extract was achieved, but on-line spectra were readily distinguishable and could be unambiguously assigned. The results are in agreement with analyses by gas chromatography-mass spectrometry (GC-MS). Thus, this method, which was found to be accurate, sensitive and rapid, has the potential for use as a reliable complementary method to GC-MS in such analyses. [source] Toxicity of methyl tert butyl ether to soil invertebrates (springtails: Folsomia candida, Proisotoma minuta, and Onychiurus folsomi) and lettuce (Lactuca sativa)ENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 2 2010Matthew Dodd Abstract Experiments were conducted to assess the toxicity of methyl tert butyl ether (MTBE) to three species of Collembola (Proisotoma minuta, Folsomia candida, and Onychiurus folsomi) and lettuce (Lactuca sativa L.) using an artificial Organization for Economic Cooperation and Development (OECD) soil and field-collected sandy loam and silt loam soil samples. Soil invertebrate tests were carried out in airtight vials to prevent volatilization of MTBE out of the test units and to allow for direct head-space sampling and gas chromatography-mass spectrometry (GC-MS) analysis for residual MTBE. The use of the airtight vial protocol proved to be very successful, in that the measured MTBE concentrations at the beginning of the experiments were within 95% of nominal concentrations. The test methods used in this study could be used to test the toxicity of other volatile organic compounds to Collembola. The soil invertebrates tested had inhibitory concentration (ICx) and lethal concentration (LCx) values that ranged from 242 to 844 mg MTBE/kg dry soil. When the three test species of Collembola were tested under identical conditions in the artificial OECD soil, O. folsomi was the most sensitive collembolan, with a median inhibitory concentration (IC50; reproduction) of 296 mg MTBE/kg dry soil. The most sensitive endpoint for lettuce was an IC50 for root length of 81 mg MTBE/kg dry soil after 5 d of germination in OECD soil. Data on the loss of MTBE from the three test soils over time indicated that MTBE was retained in the silt loam soil longer than in either the sandy loam or the artificial OECD soil. Environ. Toxicol. Chem. 2010;29:338,346. © 2009 SETAC [source] Bioavailability and biodegradation of nonylphenol in sediment determined with chemical and bioanalysis,ENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 4 2008Jasperien de Weert Abstract The surfactant nonylphenol (NP) is an endocrine-disrupting compound that is widely spread throughout the environment. Although environmental risk assessments are based on total NP concentrations, only the bioavailable fraction posses an environmental risk. The present study describes the bioavailability and biodegradability of NP over time in contaminated river sediment of a tributary of the Ebro River in Spain. The bioavailable fraction was collected with Tenax TA® beads, and biodegradation was determined in aerobic batch experiments. The presence of NP was analyzed chemically using gas chromatography-mass spectrometry and indirectly as estrogenic potency using an in vitro reporter gene assay (ER, - luc assay). Of the total extractable NP in the sediment, 95% ± 1.5% (mean ± standard error) desorbed quickly into the water phase. By aerobic biodegradation, the total extractable NP concentration and the estrogenic activity were reduced by 97% ± 0.5% and 94% ± 2%, respectively. The easily biodegradable fraction equals the potential bioavailable fraction. Only 43 to 86% of the estrogenic activity in the total extractable fraction, as detected in the ER, - luc assay, could be explained by the present NP concentration. This indicates that other estrogenic compounds were present and that their bioavailability and aerobic degradation were similar to that of NP. Therefore, we propose to use NP as an indicator compound to monitor estrogenicity of this Ebro River sediment. To what extent this conclusion holds for other river sediments depends on the composition of the contaminants and/or the nature of these sediments and requires further testing. [source] Evaluation of the ishikawa cell line bioassay for the detection of estrogenic substances from sediment extractsENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 7 2005Shinya Hashimoto Abstract This study examines the application of Ishikawa human endometrial adenocarcinoma cells to measure the estrogenic activity of fractionated extracts of sediments from Tokyo Bay, Japan. Estrogen stimulates alkaline phosphatase activity in this cell line. The results of these assays were compared with those of a yeast estrogen screen (YES) assay. The Ishikawa cell line bioassay showed higher sensitivity to 17,-estradiol (median effective concentration [EC50], 10.7 pM) than did the YES assay (EC50, 480 pM). Fractionation of sediment extracts (all samples collected from 5 sites) showed that the nonpolar fraction was poisonous to yeast cells; the estrogenic activity of this fraction, therefore, could not be measured by YES. However, the nonpolar fraction did not kill the Ishikawa cells. The 17,-estradiol-equivalent values of 15 extracts (3 fractions from each of 5 sediment samples) ranged from 5.7 to 697 pg/g dry weight according to the Ishikawa cell line bioassay. Chemical analysis using gas chromatography-mass spectrometry revealed that the highest concentrations of endocrine-disrupting chemicals were observed at the sampling station near the sewage treatment plant. The results support that the Ishikawa cell line bioassay is suitable for measuring the estrogenic activity of sediment samples. [source] Bioluminescence inhibition assays for toxicity screening of wood extractives and biocides in paper mill process watersENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 2 2004Anna Rigol Abstract The risk associated with wood extractives, biocides, and other additives in pulp and paper mill effluents was evaluated by performing a characterization of process waters and effluents in terms of toxicity and chemical analysis. The individual toxicity of 10 resin acids, two unsaturated fatty acids, and three biocides was estimated by measuring the bioluminescence inhibition with a ToxAlert® 100 system. Median effective concentration values (EC50) of 4.3 to 17.9, 1.2 to 1.5, and 0.022 to 0.50 mg/L were obtained, respectively. Mixtures of these three families of compounds showed antagonistic effects. Chemical analysis of process waters was performed by liquid chromatography-and gas chromatography-mass spectrometry. Biocides such as 2-(thiocyanome-thylthio)-benzotiazole (TCMTB) (EC50 = 0.022 mg/L) and 2,2-dibromo-3-nitrilpropionamide (DBNPA) (EC50 = 0.50 mg/L) were the most toxic compounds tested and were detected at concentrations of 16 and 59 ,g/L, respectively, in a closed-circuit recycling paper mill. Process waters from kraft pulp mills, printing paper mills, and packing board paper mills showed the highest concentration of resin acids (up to 400 ,g/L) and accounted for inhibition percentages up to 100%. Detergent degradation products such as nonylphenol (NP) and octylphenol (OP) and the plasticizer bisphenol A (BPA) were also detected in the waters at levels of 0.6 to 10.6, 0.3 to 1.4, and 0.7 to 187 ,g/L, respectively. However, once these waters were biologically treated, the concentration of detected organic compounds diminished and the toxicity decreased in most cases to values of inhibition lower than 20%. [source] ,, ,-Unsaturated sulfophenylcarboxylates as degradation intermediates of linear alkylbenzenesulfonates: Evidence for ,-oxygenation followed by ,-oxidations by liquid chromatography-mass spectrometryENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 1 2002Peter Eichhorn Abstract Liquid chromatography with an electrospray interface to a mass spectrometer (LC-ES-MS) and LC-ES coupled to a tandem MS (LC-ES-MS/MS) were used to detect and identify intermediates excreted transiently during the aerobic degradation of linear alkylbenzenesulfonates (LAS) in fixed-bed bioreactors (FBBR). The inoculum for the FBBR was the microflora of the River Rhine, Germany. Two major phenomena were observed on the addition of 100 mg/L LAS to the system, sorption and then biodegradation. Disappearance due to sorption was followed in an inhibited FBBR. Biodegradation of LAS started on day 7 and was accompanied by the transient excretion of intermediates, which were later largely degraded. We detected not only the sulfophenylcarboxylates (SPCs) observed previously but also the ,, ,-unsaturated SPCs (SPC-2H), which have not been reported before. Experiments with the (4-sulfophenyl)dodecanes (C12-LAS), which had minor contaminants of C11-LAS, showed C12-, C10-, C8-, C6-, and C4-SPCs when LAS was degraded as well as traces of C9-, C7-, and C5-SPCs. Signals from the SPC-2H species were usually some 10% of those from the corresponding SPCs. Samples from these experiments were also examined by gas chromatography-mass spectrometry (GC-MS), but no desulfonated intermediates were detected. We interpret the data to mean that the only attack on LAS was by ,-oxygenation; there was no visible initial desulfonation. The products of ,-oxygenation were oxidized to the corresponding SPC and subject to ,-oxidation, as evidenced not only by the pattern of C-2 units in the excreted SPCs but also in the corresponding series of SPC-2H, representing the intermediates in ,-oxidation. [source] Metabolism of cholesterol ester of apolipoprotein B100-containing lipoproteins in dogs: evidence for disregarding cholesterol ester transferEUROPEAN JOURNAL OF CLINICAL INVESTIGATION, Issue 8 2004E. Bailhache Abstract Background, It has been shown that dogs exhibit no cholesterol ester transfer protein (CETP) activity in vitro, in contrast to humans. The aim of our study was to determine modalities of in vivo plasma cholesterol ester turnover in this species, using a kinetic approach with stable isotopes. Materials and methods, Kinetics of very low-density lipoprotein (VLDL) and low-density lipoprotein (LDL) were studied in seven adult male Beagle dogs using a dual isotope approach through endogenous labelling of both their cholesterol moiety and their protein moiety. A primed constant infusion of both [1,213C]acetate and [5,5,5- 2H3]leucine enabled us to obtain measurable deuterium enrichments by gas chromatography-mass spectrometry for plasma leucine and apoB100, as well as measurable 13C enrichment by gas chromatography-combustion-isotopic ratio mass spectrometry for unesterified cholesterol and cholesterol ester in the VLDL and LDL. Two identical multicompartmental models (SAAM II) were used together for the analysis of tracer kinetics' data of proteins and cholesterol. Results, Characterization of the apoB100-containing lipoprotein cholesterol ester model allowed determination of kinetic parameters of VLDL and LDL cholesterol ester metabolism. We succeeded in modelling VLDL and LDL cholesterol ester metabolism and apoB100 metabolism simultaneously. Fractional catabolic rate (FCR) of apoB100 and CE had the same values. Introducing cholesterol ester transfer between lipoproteins in the model did not significantly improve the fit. Total VLDL FCR was 2·97 ± 01·47 h,1. Approximately one-quarter corresponded to the direct removal of VLDL (0·81 ± 00·34 h,1) and the remaining three-quarters corresponded to the fraction of VLDL converted to LDL, which represented a conversion of VLDL into LDL of 2·16 ± 01·16 h,1. Low-density lipoproteins were produced exclusively from VLDL conversion and were then removed (0·031 ± 0·004 h,1) from plasma. Conclusion, These kinetic data showed that VLDL cholesterol ester and LDL cholesterol ester metabolism followed VLDL and LDL apoB100 metabolism, and that consequently there is no in vivo transfer of cholesterol ester in dogs. [source] Characterization of volatile compounds and triacylglycerol profiles of nut oils using SPME-GC-MS and MALDI-TOF-MSEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 2 2009Stefanie Bail Abstract Several nut oil varieties mainly used as culinary and overall healthy food ingredients were subject of the present study. Headspace solid-phase microextraction combined with gas chromatography-mass spectrometry was employed in order to determine the qualitative composition of volatile compounds. Furthermore, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry was used in order to assess the profiles and relative composition of the prevalent triacylglycerols (TAG) within the oils. The headspace of the majority of oil samples was dominated by high contents of acetic acid (up to 42%) and hexanal (up to 32%). As nut oils are typically gained by cold-pressing from previously roasted nuts, characteristic pyrazine derivatives as well as degradation products of long-chain fatty acids were detected. TAG analysis of these oils revealed a quite homogeneous composition dominated by components of the C52 and C54 group composed mainly of oleic (18:1), linoleic (18:2), stearic (18:0) and palmitic (16:0) acid residues representing together between 65 and 95% of the investigated nut oils. The TAG profiles showed characteristic patterns which can be used as ,fingerprints' of the genuine oils. Nut oils exhibiting quite similar fatty acid composition (e.g. hazelnut, pistachio and beech oil) could be clearly discriminated based on TAG showing significant differences between the oils. [source] Geometrical isomerisation of eicosapentaenoic and docosahexaenoic acid at high temperaturesEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 7 2006Svein A. Mjøs Abstract Concentrates of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) were heated at 140,240,°C for 2,8,h under nitrogen. The trans isomers were analysed by gas chromatography-mass spectrometry on a BPX-70 cyanopropyl column. All geometrical isomers of EPA and DHA with one trans double bond were observed. The rate constants (k) for the isomerisation of the all- cis isomers were calculated and found to be higher than previously reported for linoleic acid and ,-linolenic acid. Arrhenius plots showed a linear relationship between ln,k and the reciprocal absolute temperature above 180,°C. The distribution patterns of isomers with one trans double bond are approximately constant up to a degree of isomerisation of 25%. The degree of isomerisation can therefore be estimated from selected trans peaks. [source] EVOLUTION OF REPRODUCTIVE STRATEGIES IN THE SEXUALLY DECEPTIVE ORCHID OPHRYS SPHEGODES: HOW DOES FLOWER-SPECIFIC VARIATION OF ODOR SIGNALS INFLUENCE REPRODUCTIVE SUCCESS?EVOLUTION, Issue 6 2000Manfred Ayasse Abstract The orchid Ophrys sphegodes Miller is pollinated by sexually excited males of the solitary bee Andrena nigroaenea, which are lured to the flowers by visual cues and volatile semiochemicals. In O. sphegodes, visits by pollinators are rare. Because of this low frequency of pollination, one would expect the evolution of strategies that increase the chance that males will visit more than one flower on the same plant; this would increase the number of pollination events on a plant and therefore the number of seeds produced. Using gas chromatography-mass spectrometry (GC-MS) analyses, we identified more than 100 compounds in the odor bouquets of labellum extracts from O. sphegodes; 24 compounds were found to be biologically active in male olfactory receptors based on gas chromatography with electroantennographic detection (GC-EAD). Gas chromatography (GC) analyses of odors from individual flowers showed less intraspecific variation in the odor bouquets of the biologically active compounds as compared to nonactive compounds. This can be explained by a higher selective pressure on the pollinator-attracting communication signal. Furthermore, we found a characteristic variation in the GC-EAD active esters and aldehydes among flowers of different stem positions within an inflorescence and in the n-alkanes and n-alkenes among plants from different populations. In our behavioral field tests, we showed that male bees learn the odor bouquets of individual flowers during mating attempts and recognize them in later encounters. Bees thereby avoid trying to mate with flowers they have visited previously, but do not avoid other flowers either of a different or the same plant. By varying the relative proportions of saturated esters and aldehydes between flowers of different stem positions, we demonstrated that a plant may take advantage of the learning abilities of the pollinators and influence flower visitation behavior. Sixty-seven percent of the males that visited one flower in an inflorescence returned to visit a second flower of the same inflorescence. However, geitonogamy is prevented and the likelihood of cross-fertilization is enhanced by the time required for the pollinium deposited on the pollinator to complete its bending movement, which is necessary for pollination to occur. Cross-fertilization is furthermore enhanced by the high degree of odor variation between plants. This variation minimizes learned avoidance of the flowers and increases the likelihood that a given pollinator would visit several to many different plants within a population. [source] Characterization and Variability of Endotoxin and 3-Hydroxy Fatty Acids in an Office Building During a Particle Intervention StudyINDOOR AIR, Issue 1 2000Cynthia J. Hines Abstract Air and dust samples were collected on two floors of an office building during a double-blind particle intervention study to examine spatial and temporal variability of airborne endotoxin over a period of weeks, and to characterize endotoxin activity and lipopolysaccharide (LPS) content in carpet and chair dust. Air samples were collected on multiple days within and across weeks. Dust samples were collected from carpets and chairs one day per week for three weeks. Endotoxin was measured using a Limulus assay. Dust samples were analyzed for LPS by determination of 3-hydroxy fatty acids (3-OHFAs) using gas chromatography-mass spectrometry. The geometric mean (geometric standard deviation) for 96 indoor air samples was 0.24 (1.6) EU/m3. Significant within-floor spatial variation of airborne endotoxin was found (P<0.0001, n=80). Temporal variability of airborne endotoxin was not significant across weeks. Mean (±SD) endotoxin levels in carpet dust (59±9.3 EU/mg dust, n=12) and in chair dust (38±7.7 EU/mg dust, n=10) were significantly different (P<0.001). Carbon chain length-dependent differences in 3-OHFA levels by dust source and floor were found. Enhanced air filtration did not significantly affect airborne endotoxin (P=0.62); however, total dust mass and total endotoxin in carpet dust samples increased significantly after enhanced surface cleaning (P<0.01). These findings suggest that spatial variability, dust source, and surface cleaning may influence building occupant exposures to endotoxin., [source] Breath gas aldehydes as biomarkers of lung cancerINTERNATIONAL JOURNAL OF CANCER, Issue 11 2010Patricia Fuchs Abstract There is experimental evidence that volatile substances in human breath can reflect presence of neoplasma. Volatile aldehydes were determined in exhaled breath of 12 lung cancer patients, 12 smokers and 12 healthy volunteers. Alveolar breath samples were collected under control of expired CO2. Reactive aldehydes were transformed into stable oximes by means of on-fiber-derivatization (SPME-OFD). Aldehyde concentrations in the ppt and ppb level were determined by means of gas chromatography-mass spectrometry (GC-MS). Exhaled concentrations were corrected for inspired values. Exhaled C1,C10 aldehydes could be detected in all healthy volunteers, smokers and lung cancer patients. Concentrations ranged from 7 pmol/l (161 pptV) for butanal to 71 nmol/l (1,582 ppbV) for formaldehyde. Highest inspired concentrations were found for formaldehyde and acetaldehyde (0,55 nmol/l and 0,13 nmol/l, respectively). Acetaldehyde, propanal, butanal, heptanal and decanal concentrations showed no significant differences for cancer patients, smokers and healthy volunteers. Exhaled pentanal, hexanal, octanal and nonanal concentrations were significantly higher in lung cancer patients than in smokers and healthy controls (ppentanal = 0.001; phexanal = 0.006; poctanal = 0.014; pnonanal = 0.025). Sensitivity and specificity of this method were comparable to the diagnostic certitude of conventional serum markers and CT imaging. Lung cancer patients could be identified by means of exhaled pentanal, hexanal, octanal and nonanal concentrations. Exhaled aldehydes reflect aspects of oxidative stress and tumor-specific tissue composition and metabolism. Noninvasive recognition of lung malignancies may be realized if analytical skills, biochemical knowledge and medical expertise are combined into a joint effort. [source] Chemical composition and inhibitory effect of essential oil and organic extracts of Cestrum nocturnum L. on food-borne pathogensINTERNATIONAL JOURNAL OF FOOD SCIENCE & TECHNOLOGY, Issue 6 2009Sharif M. Al-Reza Summary In this study, we examined the chemical compositions of essential oil and tested the efficacy of oil and organic extracts of Cestrum nocturnum L. against food-borne pathogens. The chemical compositions of the oil was analysed by gas chromatography-mass spectrometry (GC-MS). Forty-seven compounds representing 93.28% of the total oil were identified. The oil [5 ,L of 1:5 (v/v) dilution of oil with methanol] and organic extracts of hexane, chloroform, ethyl acetate and methanol (300 ,g per disc) of C. nocturnum displayed a great potential of antibacterial activity against Staphylococcus aureus (ATCC 6538 and KCTC 1916), Listeria monocytogenes (ATCC 19166 and ATCC 15313), Bacillus subtilis ATCC 6633, Pseudomonas aeruginosa KCTC 2004, Salmonella typhimurium KCTC 2515 and Escherichia coli ATCC 8739. Also the oil had strong detrimental effect on the viable count of the tested bacteria. The results obtained from this study may contribute to the development of new antimicrobial agents with potential applications in food industries as natural preservatives to control food-borne pathogens. [source] The Aerobic Oxidative Cleavage of Lignin to Produce Hydroxyaromatic Benzaldehydes and Carboxylic Acids via Metal/Bromide Catalysts in Acetic Acid/Water MixturesADVANCED SYNTHESIS & CATALYSIS (PREVIOUSLY: JOURNAL FUER PRAKTISCHE CHEMIE), Issue 3 2009Walt Partenheimer Abstract Roughly 30% of all woody plants is composed of lignin. Five different lignin samples, from wood and bagasse, were oxidized in air with a cobalt/manganese/zirconium/bromide (Co/Mn/Zr/Br) catalyst in acetic acid as a function of time, temperature, pressure, and lignin and catalyst concentrations. 18 products were identified via gas chromatography-mass spectrometry (GC/MS). The most valuable products from lignin were 4-hydroxybenzaldehyde, 4-hydroxybenzoic acid, 4-hydroxy-3-methoxybenzaldehyde (vanillin), 4-hydroxy-3-methoxybenzoic acid (vanillic acid), 4-hydroxy-3,5-dimethoxybenzaldehyde (syringaldehyde) and 4-hydroxy-3,5-dimethoxybenzoic acid (syringic acid). 10.9,wt% of the lignin was converted to the aromatic products. By the use of model compounds we demonstrate that 1) the presence of the phenolic functionality on an aromatic ring does inhibit the rate of reaction but that the alkyl group on the ring still does oxidize to the carboxylic acid, 2) that the masking of phenol by acetylation occurs at a reasonable rate in acetic acid, 3) that the alkyl group of the masked phenol does very readily oxidize, 4) that an acetic anhydride/acetic acid mixture is a good oxidation solvent and 5) that a two-step acetylation/oxidation to the carboxylic acid is feasible. [source] Onion aphid (Neotoxoptera formosana) attractants, in the headspace of Allium fistulosum and A. tuberosum leavesJOURNAL OF APPLIED ENTOMOLOGY, Issue 1 2007M. Hori Abstract:, Attractancy of Allium fistulosum L. and Allium tuberosum Rottl. to adult apterae of the onion aphid, Neotoxoptera formosana (Takahashi), an oligophagous aphid pest of Allium crops, was investigated with a Y-tube olfactometer. The aphids were significantly attracted to both A. fistulosum and A. tuberosum. The headspace components of both plants were extracted with solid-phase microextraction (SPME) and analysed by gas chromatography-mass spectrometry (GC-MS). The main volatile components of A. fistulosum were dipropyl disulphide (relative contents: 67%), 1-propenyl propyl disulphide (23%) and dipropyl trisulphide (6%). In the headspace of A. tuberosum, diallyl disulphide was detected as the main component (58%). Attractancy of dipropyl disulphide, dipropyl trisulphide and diallyl disulphide to the aphids was examined with the Y-tube olfactometer. The aphids were significantly attracted to dipropyl trisulphide and diallyl disulphide at a concentration of 0.01%. Dipropyl disulphide did not significantly attract the aphids at any concentrations tested. It was revealed that attractancy of A. fistulosum and A. tuberosum was caused by dipropyl trisulphide and diallyl disulphide, respectively. The findings suggest that N. formosana uses these sulphur compounds, characteristic components of Allium plants, as olfactory cues to find the host plants. [source] Biodegradation of disperse textile dye Brown 3REL by newly isolated Bacillus sp.JOURNAL OF APPLIED MICROBIOLOGY, Issue 1 2008Abstract Aims:, To isolate the potential micro-organism for the degradation of textile disperse dye Brown 3 REL and to find out the reaction mechanism. Methods and Results:, 16S rDNA analysis revealed an isolate from textile effluent contaminated soil as Bacillus sp. VUS and was able to degrade (100%) dye Brown 3REL within 8 h at static anoxic condition. A significant increase in the activities of lignin peroxidase, laccase and NADH-DCIP reductase was observed up to complete decolourization of Brown 3REL. The optimum temperature required for degradation was 40°C and pH 6·5,12·0. Phyto-toxicity and chemical oxygen demand revealed nontoxic products of dye degradation. The biodegradation was monitored by UV,VIS, FTIR spectroscopy and HPLC. The final products 6,8-dichloro-quinazoline-4-ol and cyclopentanone were characterized by gas chromatography-mass spectrometry. This Bacillus sp. VUS also decolourized (80%) textile dye effluent within 12 h. Conclusions:, This study suggests that Bacillus sp. VUS could be a useful tool for textile effluent treatment. Significance and Impact of the Study:, The newly isolated Bacillus sp. VUS decolourized 16 textile dyes and textile dye effluent also. It achieved complete biodegradation of Brown 3REL. Phytotoxicity study demonstrated no toxicity of the biodegraded products for plants with respect to Triticum aestivum and Sorghum bicolor. [source] Adrenarche and Bone Modeling and Remodeling at the Proximal Radius: Weak Androgens Make Stronger Cortical Bone in Healthy Children,JOURNAL OF BONE AND MINERAL RESEARCH, Issue 8 2003Thomas Remer Abstract Adrenarche, the physiological increase in adrenal androgen secretion, may contribute to better bone status. Proximal radial bone and 24-h urinary steroid hormones were analyzed cross-sectionally in 205 healthy children and adolescents. Positive adrenarchal effects on radial diaphyseal bone were observed. Obviously, adrenarche is one determinant of bone mineral status in children. Introduction: Increased bone mass has been reported in several conditions with supraphysiological adrenal androgen secretion during growth. However, no data are available for normal children. Therefore, our aim was to examine whether adrenal androgens within their physiological ranges may be involved in the strengthening of diaphyseal bone during growth. Methods: Periosteal circumference (PC), cortical density, cortical area, bone mineral content, bone strength strain index (SSI), and forearm cross-sectional muscle area were determined with peripheral quantitative computed tomography (pQCT) at the proximal radial diaphysis in healthy children and adolescents. All subjects, aged 6,18 years, who collected a 24-h urine sample around the time of their pQCT analysis (100 boys, 105 girls), were included in the present study, and major urinary glucocorticoid (C21) and androgen (C19) metabolites were quantified using gas chromatography-mass spectrometry. Results and Conclusions: We found a significant influence of muscularity, but not of hormones, on periosteal modeling (PC) before the appearance of pubic hair (prepubarche). Similarly, no influence of total cortisol secretion (C21) was seen on the other bone variables. However, positive effects of C19 on cortical density (p < 0.01), cortical area (p < 0.001), bone mineral content (p < 0.001), and SSI (p < 0.001),reflecting, at least in part, reduction in intracortical remodeling,were observed in prepubarchal children after muscularity or age had been adjusted for. This early adrenarchal contribution to proximal radial diaphyseal bone strength was further confirmed for all cortical variables (except PC) when, instead of C19 and C21, specific dehydroepiandrosterone metabolites were included as independent variables in the multiple regression model. During development of pubic hair (pubarche), muscularity and pubertal stage rather than adrenarchal hormones seemed to influence bone variables. Our study shows that especially the prepubarchal increase in adrenal androgen secretion plays an independent role in the accretion of proximal radial diaphyseal bone strength in healthy children. [source] CHRACTERIZATION AND 1,1-DIPHENYL-2-PICRYLHYDRAZYL RADICAL SCAVENGING ACTIVITY OF METHANOL AND SUPERCRITICAL CARBON DIOXIDE EXTRACTS FROM LEAVES OF ADINANDRA NITIDAJOURNAL OF FOOD BIOCHEMISTRY, Issue 4 2008BENGUO LIU ABSTRACT Leaves of Adinandra nitida are consumed in southern China as health tea (Shiyacha) and as herbal medicine. In this study, the methanol and supercritical fluid extracts from leaves of A. nitida were obtained by traditional solvent extraction and supercritical carbon dioxide extraction, respectively. Both the extracts showed high 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity. By using ultraviolet-visible spectrometry (UV), infrared spectrometry (IR), nuclear magnetic resonance, electrospray ionization mass spectrometry (ESI-MS), high-performance liquid chromatography-ESI/MS, the main bioactive constituents in the methanol extract (ME) were identified as camellianin A, camellianin B, apigenin. By analysis of gas chromatography-mass spectrometry, a total of 16 compounds accounting for 98.79% of the supercritical fluid extract (SFE) were identified as ,-sitosterol, vitamin E, ,-tocopherol and so on. These compounds found in ME and SFE could contribute to the DPPH radical scavenging performance of the extracts in this study. PRACTICAL APPLICATION Adinandra nitida is a kind of particular wild plant in South China. Few reports have been published about it in the world. In this study, the methanol and supercritical fluid extracts from leaves of A. nitida were respectively obtained by two kinds of industrially significant methods, traditional solvent extraction and supercritical carbon dioxide extraction. By using ultraviolet-visible spectrometry (UV), infrared spectrometry (IR), nuclear magnetic resonance, electrospray ionization mass spectrometry (ESI-MS), high-performance liquid chromatography-ESI/MS, gas chromatography-MS, the main bioactive constituents in the two extracts were identified as flavonoids and plant sterols. Both the extracts showed high 1,1-diphenyl-2-picrylhydrazyl radical scavenging activity and this activity of the flavonoid-rich methanol extract was 10 times more than that of butylated hydroxytoluene. These results showed that leaves of A. nitida is a new kind of natural antioxidant-rich, flavonoid-rich plant source with great commercial interest in the food and phytopharmaceutical market. [source] ANTIBACTERIAL ACTIVITY AND CHEMICAL CONSTITUTIONS OF OLEA EUROPAEA L. LEAF EXTRACTSJOURNAL OF FOOD PROCESSING AND PRESERVATION, Issue 3 2010MIHRIBAN KORUKLUOGLU ABSTRACT The in vitro antimicrobial activity of aqueous, acetone, diethyl ether and ethyl alcohol extracts of olive leaves (Olea europaea L.) was studied. The aqueous extract of olive leaves had no antibacterial effect against the test microorganisms, whereas acetone extract showed inhibitory effect on Salmonella enteritidis, Bacillus cereus, Klebsiella pneumoniae, Escherichia coli, Enterococcus faecalis, Streptococcus thermophilus and Lactobacillus bulgaricus. Furthermore, the antimicrobial activities of some phenolic compounds against microorganisms were tested. The most effective compound was found to be oleuropein while syringic acid was found ineffective. The characterization of phenolic compounds in different extracts determined by high performance liquid chromatography-air pressure chemical ionization-mass spectrometry detector (HPLC-APCI-MSD GC-MS) gas chromatography-mass spectrometry (GC-MS). The acetone and the ethyl alcohol extracts had the most and the least oleuropein content, respectively. PRACTICAL APPLICATIONS In recent years the extracts of many plant species have become popular, and attempts to characterize their bioactive principles have gained speed for many pharmaceutical and food-processing applications. Especially, antimicrobial properties of plants have revived as a consequence of current problems associated with the use of chemical preservatives. Because of consumers' negative perspectives of synthetic preservatives, attention is shifting toward natural alternatives. The findings suggest that olive leaf extracts and their phenolic compounds have good potential as antibacterial substances in food preservation as they may be more acceptable to consumers and the regulatory agencies in comparison with synthetic chemical compounds. [source] CHEMICAL CHARACTERIZATION AND ANTIFUNGAL ACTIVITY OF ORIGANUM ONITES L. ESSENTIAL OILS AND EXTRACTSJOURNAL OF FOOD SAFETY, Issue 1 2009MIHRIBAN KORUKLUOGLU ABSTRACT Essential oils (EOs) and extracts (methanol, acetone and diethyl ether) of fresh and dried oregano (Origanum onites L.) were used to determine the antifungal effect on Alternaria alternata, Aspergillus flavus (two strains), Aspergillus niger (two strains), Aspergillus parasiticus, Fusarium semitectum, Fusarium oxysporum, Mucor racemosus and Penicillium roqueforti by disk diffusion methods. Minimum inhibitory concentration (MIC) and minimum fungicidal concentration (MFC) of all samples were determined. The antifungal activity of the fresh herb was greater than that of the dried herb. MIC values for fresh and dried methanol extracts were 150,950 µg/mL and 750,950 µg/mL, respectively. MFC values for methanol extracts were determined between 300 and 1200 µg/mL for fresh oregano and between 750 and 1100 µg/mL for dried oregano. The EOs of fresh and dried oregano totally inhibited test fungi. EOs produced the lowest MIC and MFC values: 8.5 µg/mL and 9.0 µg/mL, respectively (P < 0.005). The highest extract activity was exhibited by fresh oregano against A. alternata (24 mm) followed by P. roqueforti (20 mm). The greatest total antifungal effect was observed from methanol extracts. The chemical composition of fresh oregano EO and extracts was examined using gas chromatography-mass spectrometry (GC-MS). Over 80 volatiles were detected, of which 42 were positively identified by matching both MS fragmentation patterns with standardized retention characteristics. p-Cymene, thymol and carvacrol were the most prominent, followed by ,-pinene, camphor and borneol. PRACTICAL APPLICATIONS In the past decade interest in natural antimicrobial plant extracts has been growing. Various plants have historically been used for the purposes of food preservation and flavor enhancement as well as medicinal purposes. An example is oregano, the leafy part of the plant belonging to the Labiatae family. It has been used to improve the flavor and the organoleptic properties of many foods from numerous cultures. It has also been used to prolong the storage life of foods probably because of antifungal properties. The preservative nature of fresh oregano has been employed in many food applications, including meat and fish products, as well as in pharmaceuticals, alternative medicines and natural therapies. [source] Characterization of Fish Sauce Aroma-Impact Compounds Using GC-MS, SPME-Osme-GCO, and Stevens' Power Law ExponentsJOURNAL OF FOOD SCIENCE, Issue 4 2008A.J. Pham ABSTRACT:, The objectives of this study were to characterize volatile compounds and to determine the characteristic aromas associated with impact compounds in 4 fish sauces using solid-phase micro-extraction, gas chromatography-mass spectrometry, Osme, and gas chromatography olfactometry (SPME-Osme-GCO) coupled with Stevens' Power Law. Compounds were separated using GCMS and GCO and were identified with the mass spectral database, aroma perceived at the sniffing port, retention indices, and verification of compounds by authentic standards in the GCMS and GCO. Aromas that were isolated and present in all 4 fish sauce samples at all concentrations included fishy (trimethylamine), pungent and dirty socks (combination of butanoic, pentanoic, hexanoic, and heptanoic acids), cooked rice and buttery popcorn (2,6-dimethyl pyrazine), and sweet and cotton candy (benzaldehyde). All fish sauces contained the same aromas as determined by GCO and GCMS (verified using authentic standard compounds), but the odor intensity associated with each compound or group of compounds was variable for different fish sauce samples. Stevens' Power Law exponents were also determined using this analytical technique, but exponents were not consistent for the same compounds that were found in all fish sauces. Stevens' Power Law exponents ranged from 0.14 to 0.37, 0.24 to 0.34, 0.09 to 0.21, and 0.10 to 0.35 for dirty socks, fishy, buttery popcorn, and sweet aromas, respectively. This demonstrates that there is variability in Stevens' Power Law exponents for odorants within fish sauce samples. [source] | |||||||||||||||||||||||||