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At least 397 records · Page 22Linked to original sources

PubMed2000

Determination of main and minor components of silicon based materials by a combustion with elemental fluorine. Separation of gaseous fluorination products by carrier gas distillation and gas mass spectrometry

For the determination of main and minor components in silicon-based ceramic powders, a decomposition by a combustion with elemental fluorine and separation of the volatile fluorination products by a carrier-gas distillation with a subsequent detection by quadrupole mass spectrometry is described. The necessity and success of the separation step is demonstrated for the determination of boron as a minor constituent in SiC, where the spectral interferences of silicon on the boron signals are decreased considerably. The method developed is shown to be directly applicable to determination of silicon in Si3N4, SiC, and SiO2. The determination of nitrogen in Si3N4 requires additional effort, to separate nitrogen from the excess of fluorine. For the determination of boron, a complete mobilization of BF3 is assured by the presence of an adequate amount of GeF4. Analysis results obtained with different types of calibration show a precision of 30 microg for boron at the milligram-per-gram level and a precision between 0.5 and 2% (m/m) for the main components, silicon and nitrogen. Within these standard deviations, the results agree well with the values expected from the stoichiometry, with the results for silicon and boron obtained by wet chemical decomposition and slurry techniques in combination with ICP-OES and with the results for nitrogen obtained by carrier gas heat extraction.

Journal Article↗

PubMed2003

Analysis of volatile compounds of taperebá (Spondias mombin L.) and cajá (Spondias mombin L.) by simultaneous distillation and extraction (SDE) and solid phase microextraction (SPME).

Volatile compounds of cajá and taperebá fruits, both classified as Spondias mombin, but from different geographic origins, were extracted (and analyzed) using solid phase microextraction (SPME) and simultaneous distillation and extraction (SDE). Forty-eight compounds were identified in taperebá and 47 in cajá by SPME using a DVB/CAR/PMDS fiber. (E)-Caryophyllene (18.7%), ethyl butyrate (10.0%), and ethyl hexanoate (7.0%) were the most abundant components in taperebá volatiles extracted by SPME, whereas myrcene (41.1%) and beta-phellandrene (8.5%) were the major compounds in cajá. In the taperebá SDE extract, 46 substances were identified, and (Z)-caryophyllene (13.2%) and limonene (9.5%) were predominant. From the 42 substances found in the SDE extract of cajá, the major components were myrcene (38.0%) and p-cymene (6.2%). The two fruits showed similar chromatograms upon the use of SDE and SPME. These methods made it possible to determine 30 identical components in both fruits by using SDE and 32 by using SPME.

Anacardiaceae↗

PubMed2004

Aroma characteristics of stored tobacco cut leaves analyzed by a high vacuum distillation and canister system.

An extraction method using a high vacuum distillation extraction apparatus coupled to a canister was newly developed for the analysis and sensory test of tobacco leaf volatiles. We extended the application of the canister that is used in environmental analysis, to the extraction of the aroma components in tobacco leaves. The volatile components with vapor pressures higher than 0.1 mmHg were easily evaporated under decompression and then trapped into the vacuumed canister. After the collection of volatiles, the canister was pressurized by a slow stream of inert gas in order to emit the whole aroma under a controlled flow. Applying a preconcentrator--gas chromatography/mass spectrometry (GC/MS) and sensory test to the headspace gas components, the aroma alteration between 0 and 2 weeks of storage was simultaneously or individually evaluated. As a result, after the storage, alcohols such as 1-hexanol, linalool, and benzyl alcohol decreased significantly. The amount of carotenoid derivatives that have the characteristic tobacco leaf aroma had not changed. Sensory evaluation of the same headspace gas with that used for GC/MS demonstrated the alternation of the aroma quality before and after storage. The main changes were the decrease of greenness and smoothness in aroma and the decrease of ethylbenzene, 2-pentylfuran, 1-hexanol, benzaldehyde, and linalool concentrations.

Adult↗

PubMed2005

Volatile components and key odorants of fennel (Foeniculum vulgare Mill.) and thyme (Thymus vulgaris L.) oil extracts obtained by simultaneous distillation-extraction and supercritical fluid extraction.

Volatile oil extracts of fennel seeds (Foeniculum vulgare Mill.) and thyme leaves (Thymus vulgaris L.) were obtained by simultaneous distillation-extraction (SDE) and supercritical fluid extraction (SFE) and analyzed by gas chromatography-mass spectrometry (GC-MS). In general, fennel oil extracted by SDE and SFE showed similar compositions, with trans-anethole, estragole, and fenchone as the main components. In contrast, thymol and p-cymene, the most abundant compounds in thyme leaves, showed big differences, with generally higher amounts of monoterpenes obtained by SDE. However, in this case, the differences between the extracts were higher. Key odorants of fennel seeds determined by gas chromatography-olfactometry (GC-O) showed similar patterns when applying SDE and SFE. trans-Anethole (anise, licorice), estragole (anise, licorice, sweet), fenchone (mint, camphor, warm), and 1-octen-3-ol (mushroom) were the most intense odor compounds detected in fennel extracts. Thymol and carvacrol, with oregano, thyme, and spicy notes, were identified as key compounds contributing to the aroma of thyme leaves.

Chromatography, Gas↗

PubMed2006

Liquid chromatography/mass spectrometry and liquid chromatography/nuclear magnetic resonance as complementary analytical techniques for unambiguous identification of polymethoxylated flavones in residues from molecular distillation of orange peel oils (Citrus sinensis).

Liquid chromatography/mass spectrometry and liquid chromatography/nuclear magnetic resonance techniques with ultraviolet/diode array detection were used as complementary analytical tools for the reliable identification of polymethoxylated flavones in residues from molecular distillation of cold-pressed peel oils of Citrus sinensis. After development of a liquid chromatographic separation procedure, the presence of several polymethoxy flavones such as sinensetin, nobiletin, tangeretin, quercetogetin, heptamethoxyflavone, and other derivatives was unambiguously confirmed. In addition, proceranone, an acetylated tetranortriterpenoid with limonoid structure, was identified for the first time in citrus.

Chromatography, High Pressure Liquid↗

PubMed2006

Study of the influence of alcoholic fermentation and distillation on the oxygen-18/oxygen-16 isotope ratio of ethanol.

A laboratory procedure for the analysis of the oxygen-18/oxygen-16 isotope ratios of ethanol derived from sugars and fruit juices by pyrolysis-isotope ratio mass spectrometry (IRMS) has been applied to the study of isotopic fractionation induced by the isotope effects of fermentation and distillation. For both processes, an experimental model has been established to describe and explain the observed fractionation phenomena. It is shown that reproducible results can be obtained when appropriate analytical conditions are used. Moreover, the ability of ethanol to act as a reliable indicator of the (18)O/(16)O ratio of sugars in orange juice (and therefore to be used as an internal reference for detecting water addition) is demonstrated both in theory and in practice.

Alcohols↗

PubMed2005

Hydrogen bonding in alcoholic beverages (distilled spirits) and water-ethanol mixtures.

The hydrogen-bonding properties of water-ethanol of alcoholic beverages and water-ethanol mixtures of the corresponding ethanol contents were examined on the basis of OH proton NMR chemical shifts and the Raman OH stretching spectra of water and ethanol. Japanese shochu, an unaged distilled spirit of 25% (v/v) alcoholic content made from various grains, was provided for the samples; it is a high-purity spirit as it contains only small amounts of dissolved components, like typical vodka, gin, and white rum. The hydrogen-bonding structure in shochu containing some acids was found to be different from that of the water-ethanol mixture with corresponding ethanol content. It was concluded that, by the presence of small amounts of organic acids, the water-ethanol hydrogen-bonding structure was strengthened, at the same time, the proton exchange between water and ethanol molecules was promoted in shochu, compared with the water-ethanol mixture. The NMR chemical shifts of fruit cocktail drinks suggested that the hydrogen bonding of water-ethanol in the solution was developed by organic acids and (poly)phenols from fruit juices.

Alcoholic Beverages↗

PubMed2006

Discrimination of Cognacs and other distilled drinks by mid-infrared spectropscopy.

Mid-infrared spectroscopy was applied to the analysis and discrimination of Cognacs and other distilled drinks (Armagnacs, whiskies, brandies, bourbons, rums, and counterfeit products). Strong correlations were found between dry extract spectra, polyphenolic dry extract spectra, and the total polyphenol concentration of samples, notably of Cognacs. Principal component analysis applied to spectral data made it possible to emphasize the importance of dry extract data when a distinction is made between Cognacs and Armagnacs, whiskies, bourbons, and rums, and of polyphenol concentration when Cognacs, brandies, and counterfeit products are separated. Ninety-six percent of samples in the test set were correctly assigned to Cognacs and non-Cognacs by partial least-squares discriminant analysis.

Alcoholic Beverages↗

PubMed1999

Analysis of 2-methylisoborneol and geosmin in catfish by microwave distillation--solid-phase microextraction.

The semivolatile cyclic alcohols 2-methylisoborneol (MIB) and geosmin (GSM) impart muddy or musty flavors to water and food products. A rapid quantitative analytical technique has been developed whereby microwave distillation is used to remove the volatile organic compounds from a lipophilic matrix into an aqueous matrix. Solid-phase microextraction (MD-SPME) is then used to extract and concentrate the analytes, which are then desorbed in the injection port of a gas chromatograph/mass spectrometer (GC/MS) for analysis. Limits of detection are 0.01 microg/kg and limits of quantification are 0.1 microg/kg. MD-SPME is comparable in precision, requires no solvents, and is faster than current methods of analysis. This methodology allows detection of MIB and GSM at concentrations below human sensory thresholds in fish tissue.

Animals↗

PubMed2002

Distilling the essential features of a protein surface for improving protein-ligand docking, scoring, and virtual screening.

For the successful identification and docking of new ligands to a protein target by virtual screening, the essential features of the protein and ligand surfaces must be captured and distilled in an efficient representation. Since the running time for docking increases exponentially with the number of points representing the protein and each ligand candidate, it is important to place these points where the best interactions can be made between the protein and the ligand. This definition of favorable points of interaction can also guide protein structure-based ligand design, which typically focuses on which chemical groups provide the most energetically favorable contacts. In this paper, we present an alternative method of protein template and ligand interaction point design that identifies the most favorable points for making hydrophobic and hydrogen-bond interactions by using a knowledge base. The knowledge-based protein and ligand representations have been incorporated in version 2.0 of SLIDE and resulted in dockings closer to the crystal structure orientations when screening a set of 57 known thrombin and glutathione S-transferase (GST) ligands against the apo structures of these proteins. There was also improved scoring enrichment of the dockings, meaning better differentiation between the chemically diverse known ligands and a approximately 15,000-molecule dataset of randomly-chosen small organic molecules. This approach for identifying the most important points of interaction between proteins and their ligands can equally well be used in other docking and design techniques. While much recent effort has focused on improving scoring functions for protein-ligand docking, our results indicate that improving the representation of the chemistry of proteins and their ligands is another avenue that can lead to significant improvements in the identification, docking, and scoring of ligands.

Algorithms↗

PubMed2003

Vulgarone B, the antifungal constituent in the steam-distilled fraction of Artemisia douglasiana.

Antifungal activity of the steam distilled essential oil fraction of Artemisia douglasiana was detected by bioautography on silica gel TLC plates against three Colletotrichum spp. The active principle was isolated by bioassay-directed fractionation using column chromatography followed by crystallization and was characterized as vulgarone B by 1H and 13C NMR and GC-MS. Antifungal activity of vulgarone B was further evaluated using 96-well microtiter assay against Colletotrichum acatatum, C. fragariae, C. gloeosporioides, and Botrytis cinerea. In addition, the antifungal activity of vulgarone B and verbenone, and their corresponding alcohols was tested by bioautography and microtiter assay. Structure-activity studies revealed that the alpha, beta-unsaturated carbonyl functionality is a prerequisite for the antifungal activity of these mono and sesquiterpene ketones. This is the first report of antifungal activity of vulgarone B. The yield of essential oil from A. douglasiana is about 0.6-0.8% by weight of the dry material, including plant stems.

Antifungal Agents↗

PubMed1998

A partial involvement of histamine in ultrasonically nebulized distilled water-induced bronchoconstriction in guinea-pigs.

1. Inhalation of ultrasonically nebulized distilled water (UNDW) can induce bronchoconstriction only in asthmatics, but mechanisms of the response are not well known. We recently reported a guinea-pig model of UNDW-induced bronchoconstriction (UNDW-IB) in which UNDW induces bronchoconstriction when UNDW is inhaled 20 min after a challenge with aerosolized ovalbumin (OA) in passively sensitized, anaesthetized and artificially ventilated guinea-pigs. 2. To elucidate the role of histamine in the UNDW-IB, we examined the effects of antihistamines, diphenhydramine hydrochloride (DH) and chlorpheniramine maleate (CP), and measured histamine content in bronchoalveolar lavage fluid (BALF) in the animal model. 3. DH in doses of 0.1, 1.0 and 10 mg kg(-1) and CP in doses of 0.01, 0.1 and 1.0 mg kg(-1) administered intravenously 15 min after the OA challenge partially reduced the UNDW-IB at 1 and 2 min after the UNDW inhalation in a dose-dependent manner. Histamine content in BALF recovered 10 min after the UNDW inhalation following the OA provocation was significantly increased compared with that after saline inhalation and before the UNDW inhalation following the OA challenge. 4. Intravenous atropine in a dose of 0.5 mg kg(-1) or inhaled disodium cromoglycate in concentrations of 1 and 10 mg ml(-1) did not alter the UNDW-IB. 5. These results suggest that histamine is involved in part in the UNDW-IB in our animal model.

Administration, Inhalation↗

PubMed2004

Characterisation of weathered hydrocarbon wastes at contaminated sites by GC-simulated distillation and nitrous oxide chemical ionisation GC-MS, with implications for bioremediation.

An extended analytical characterisation of weathered hydrocarbons isolated from historically contaminated sites in Alberta is presented. The characterisation of soil extracts, chromatographically separated into component classes, by GC-simulated distillation and nitrous oxide (N2O) chemical ionisation (CI) GC-MS provides new insights into the composition of the residual oil at these sites, the principal partition medium for risk critical components. The combined polar and asphaltene content of representative soil extracts ranged from 40% w/w to 70% w/w of the oils encountered. An abundance of C14-C22 2-4 ring alicyclics, alkylbenzenes and benzocycloparaffins is prevalent within the saturate fractions of site soils. Implications for the partitioning of risk critical compounds at sites with weathered hydrocarbons and the practical application of bioremediation technologies are discussed.

Alberta↗

PubMed1971

Effect of electrolytes and of distilled water on antigen-antibody complexes.

Specific immune precipitates dissolve in concentrated solutions of alkali-metal halides, and of alkaline-earth-metal halides and thiocyanates. The quantity of protein dissolved depends on the nature of the antigen-antibody system, on the proportion of the antigen in the precipitate, and on the avidity of the antibody. The extent of solubilization is a function of the temperature, of the volume of solution used and of the concentration of the ions in the solution, and also depends on the nature of these ions. The dissolving power of bivalent cations is greater than that of monovalent ones, and is as follows: Mg(2+)[unk]Ba(2+)[unk]Ca(2+)[unk]Sr(2+). Antigen-antibody complexes and free antibodies, but no free antigen, are detected in supernatants of specific precipitates dissolved in solutions of electrolytes of low ionic strength. Antigen-antibody complexes, free antibodies and also free antigen are detected in supernatants of specific precipitates dissolved in solutions of electrolytes of high ionic strength. Comparable results are obtained when the electrolyte solutions are studied for their effect on the bonds formed between an antibody and its corresponding immunosorbent. Moreover, in the latter case, 50% of the fixed antibodies could be recovered by elution with distilled water.

Animals↗

PubMed1998

Role of tachykinins in distilled water-induced bronchoconstriction in guinea-pigs.

BACKGROUND: An inhalation of ultrasonically nebulized distilled water (UNDW) induces bronchoconstriction only in asthmatics, but the mechanism underlying the response is not fully understood. We recently showed that bronchoconstriction occurs immediately after UNDW is inhaled 20min after an aerosolized antigen challenge in passively sensitized guinea-pigs. OBJECTIVE: This study was conducted to examine the role of tachykinins in this response. METHODS: Passively sensitized animals were anaesthetized and artificially ventilated, and changes in pressure at the airway opening (Pao) were measured as an overall index of airway narrowing. A tachykinin NK1 and NK2 dual receptor antagonist, FK224, and a tachykinin NK1 selective antagonist, FK888, were intravenously administered 15 min after the antigen challenge. The effects of capsaicin desensitization and a neutral endopeptidase inhibitor, phosphoramidon, were also examined. RESULTS: FK224 and FK888 significantly (P < 0.05 and P < 0.05, respectively) reduced the time course curve of the increase in Pao caused by UNDW inhalation in a dose-dependent manner. The percentage increase in Pao from the preantigen challenge value at 1 min after the UNDW inhalation was 267.4+/-17.1, 358.0+/-33.7 and 412.4+/-27.6% with 10 mg/kg of FK224, 1.0 mg/kg of FK224 and vehicle, respectively, (P<0.01 between 10 mg/kg of FK224 and vehicle) and the value was 254.4+/-48.5% with 10 mg/kg of FK888, 327.1+/-57.6% with 1.0 mg/kg of FK888 and 418.5+/-39.0% with vehicle, respectively (P < 0.05 between 10 mg/kg of FK888 and vehicle). The capsaicin desensitization, but not phosphoramidon, significantly reduced the UNDW-induced increase in Pao. CONCLUSION: These results suggest that tachykinins, at least substance P, are involved in a part of the UNDW-induced bronchoconstriction in our guinea-pig model.

Animals↗

PubMed2006

Theory of "laser distillation" of enantiomers: purification of a racemic mixture of randomly oriented dimethylallene in a collisional environment.

Enantiomeric control of 1,3 dimethylallene in a collisional environment is examined. Specifically, our previous "laser distillation" scenario wherein three perpendicular linearly polarized light fields are applied to excite a set of vib-rotational eigenstates of a randomly oriented sample is considered. The addition of internal conversion, dissociation, decoherence, and collisional relaxation mimics experimental conditions and molecular decay processes. Of greatest relevance is internal conversion which, in the case of dimethylallene, is followed by molecular dissociation. For various rates of internal conversion, enantiomeric control is maintained in this scenario by a delicate balance between collisional relaxation of excited dimethylallene that enhances control and collisional dephasing, which diminishes control.

Journal Article↗

PubMed1996

Developmental toxicity of clarified slurry oil, syntower bottoms, and distillate aromatic extract administered as a single oral dose to pregnant rats.

Clarified slurry oil (CSO), syntower bottoms (STB), and distillate aromatic extract (DAE) are refinery streams produced by processing crude oil. Each of these refinery streams is rich in both hydrocarbons having carbon numbers of C20 or greater and polycyclic aromatic compounds. Available data indicate that some refinery streams are developmentally toxic (manifested primarily as increased embryolethality and growth retardation) by the dermal route of exposure. However, there is no conclusive evidence for their being teratogenic. The present studies were designed to further explore the suspected teratogenic potency of refinery streams while at the same time limiting embryolethality. To profile teratogenic effects as a function of gestation day, pregnant rats received a single oral dose (2000 mg/kg) of CSO, STB, or DAE on one of gestation days (GD) 11-14; DAE and STB were also administered on GD 15. To profile effects as a dose response function, rats received a single oral dose of CSO, DAE, or STB on GD 12 at 125, 500, and 2000 mg/kg. Control animals were similarly treated but were administered tap water. On GD 20, dams were necropsied and the fetuses evaluated for normal development. In general, evidence of maternal toxicity (i.e., decreased body weight gain, decreased thymus weight) was observed at doses greater than or equal to 500 mg/kg. For each refinery stream tested, the incidence of resorption was greatest on GD 11. A common pattern of fetal malformations was observed for all of the refinery streams tested and included cleft palate, diaphragmatic hernia, and paw and tail defects. The incidence and type of malformation observed were influenced by the gestation day of exposure. The incidences of external and skeletal malformations were greatest on GD 11 and 12 for fetuses exposed to CSO; on GD 13 and 14, the incidence of malformation was comparable for CSO- and STB-exposed fetuses. The incidence of visceral anomalies was greatest on GD 11-13 for fetuses exposed to CSO and STB; on Gestation D 14, the incidence was comparable for each of the refinery streams tested. In general, the ability to produce adverse effects on development was greatest for CSO and least for DAE. Effects produced by STB were comparable to or less severe than those observed for CSO.

Abnormalities, Drug-Induced↗

PubMed1998

Toxicity evaluation of petroleum blending streams: inhalation subchronic toxicity/neurotoxicity study of a light alkylate naphtha distillate in rats.

A 13-wk inhalation study was conducted with Sprague-Dawley CD rats (12/sex/group) were exposed by inhalation for 13 weeks to a light alkylate naphtha distillate (LAND-2, C4-C10; average molecular weight 89.2) at actual average concentrations of 0 (room air), 668, 2220, or 6646 ppm, 6 h/d, 5 d/wk; 12 additional rats/sex in the control and high dose groups were held after final exposure for a 4-wk recovery period. The highest exposure concentration was 75% of the lower explosive limit. Standard parameters of subchronic toxicity were measured throughout the study; at necropsy, organs were weighed and tissues processed for microscopic evaluation. Neurotoxicity evaluations consisted of motor activity (MA) and a functional operational battery (FOB) measured pretest, during 5, 9, and 14 wk of the study, and after the 4-wk recovery period. Whole-body perfusion and microscopic examination of selected organs and nervous tissue from the control and high dose rats were conducted at the end of exposure. No test-related mortality or effects on physical signs, body weight, or food consumption were observed. Statistically significant increases in absolute and relative kidney weights in high-exposure males correlated with microscopically observed hyaline droplet formation and renal nephropathy, effects in male rats that are not toxicologically significant for humans. Increased liver weights in both sexes at the highest dose had no microscopic correlate and appeared reversible after the 4-wk recovery period. Exposure to LAND-2 at any dose did not produce neurotoxicity measured by MA, FOB, or neuropathology. The no-observed-effects level (NOEL) for LAND-2 was 2220 ppm for subchronic toxicity and > or =26646 ppm for neurotoxicity.

Administration, Inhalation↗