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PubMed2004

A new class of platinum (II) vapochromic salts.

Luminescent chloride and hexaflurophosphate salts of Pt(Me2bzimpy)Cl+ (Me2bzimpy = 2,6-bis(1-methylbenzimidazol-2-yl)pyridine) are reported. As solids, both compounds are vapochromic, undergoing pronounced and reversible changes of color and emission in the presence of volatile organic compounds. The chloride salt responds to vapors of methanol, chloroform, ethanol, and acetonitrile, undergoing a distinct change in color from yellow to red within seconds. The PF6- salt responded selectively to acetonitrile vapor, changing from yellow to violet while sorbing 1.0 +/- 0.1 equiv. For either salt, leaving vapor-exposed samples in air for several days or heating for several minutes restored the original color. UV-visible absorption spectra and solid-state room temperature and 77 K emission spectra are reported, and the accumulated data are consistent with a decrease in Pt...Pt separation accompanying vapor sorption.

Journal Article↗

PubMed2006

Genetic damage induced by accidental environmental pollutants.

Petroleum is one of the main energy sources worldwide. Its transport is performed by big tankers following some established marine routes. In the last 50 years a total amount of 37 oil tankers have given rise to great spills in different parts of the world, Prestige being the last one. After the accident, a big human mobilisation took place in order to clean beaches, rocks and fauna, trying to reduce the environmental consequences of this serious catastrophe. These people were exposed to the complex mixture of compounds contained in the oil. This study aimed at determine the level of environmental exposure to volatile organic compounds (VOC), and the possible damage induced on the population involved in the different cleaning tasks by applying the genotoxicity tests sister chromatid exchanges (SCE), micronucleus (MN) test, and comet assay. Four groups of individuals were included: volunteers (V), hired manual workers (MW), hired high-pressure cleaner workers (HPW) and controls. The higher VOC levels were associated with V environment, followed by MW and lastly by HPW, probably due to the use of high-pressure cleaners. Oil exposure during the cleaning tasks has caused an increase in the genotoxic damage in individuals, the comet assay being the most sensitive biomarker to detect it. Sex, age and tobacco consumption have shown to influence the level of genetic damage, while the effect of using protective devices was less noticeable than expected, perhaps because the kind used was not the most adequate.

Accidents, Occupational↗

PubMed2005

Method for analysis of polar volatile trace components in aqueous samples by gas chromatography.

A new method has been developed for direct analysis of volatile polar trace compounds in aqueous samples by gas chromatography. Water samples are injected onto a short packed precolumn containing anhydrous lithium chloride. A capillary column is coupled in series with the prefractionation column for final separation of the analytes. The enrichment principle of the salt precolumn is reverse to the principles employed in conventional methods such as SPE or SPME in which a sorbent or adsorbent is utilized to trap or concentrate the analytes. Such methods are not efficient for highly polar compounds. In the LiCl precolumn concept, the water matrix is strongly retained on the hygroscopic salt, whereas polar as well as nonpolar volatile organic compounds show very low retention and are eluted ahead of the water. After transfer of the analytes to the capillary column, the retained bulk water is removed by backflushing the precolumn at elevated temperature. For direct injections of 120 microL of aqueous samples, the combined time for injection and preseparation is only 3.5 min. With this procedure, direct repetitive automated analyses of highly volatile polar compounds such as methanol or tetrahydrofuran can be performed, and a limit of quantification in the low parts-per-billion region utilizing a flame ionization detector is demonstrated.

Journal Article↗

PubMed2004

Leaching of organic contaminants from storage of reclaimed asphalt pavement.

Recycling of asphalt has been promoted by rapid increases in both the use and price of petroleum-based bitumen. Semi-volatile organic compounds in leachates from reclaimed asphalt pavement, measured in field samples and in laboratory column test, were analysed through a GC/MS screen-test methodology. Sixteen PAH (polyaromatic hydrocarbons) were also analysed in leachates from the column study. The highest concentrations of semi-volatile compounds, approximately 400 microg l(-1), were measured in field samples from the scarified stockpile. Naphthalene, butylated hydroxytoluene (BHT) and dibutyl phthalate (DBP) were the most dominant of the identified semi-volatiles. The occurrence of these compounds in urban groundwater, also indicate high emission rates and persistent structures of the compounds, making them potentially hazardous. Car exhausts, rubber tires and the asphalt material itself are all probable emission sources, determined from the organic contaminants released from the stockpiles. The major leaching mechanism indicated was dissolution of organic contaminants from the surface of the asphalt gravels. In the laboratory column test, the release of high-molecular weight and more toxic PAH was higher in the leachates after two years than at the commencement of storage. The concentrations of semi-volatiles in leachates, were also several times lower than those from the field stockpile. These results demonstrate the need to follow up laboratory column test with real field measurements.

Butylated Hydroxytoluene↗

PubMed2003

[Historical study of separation technology innovation in the field of pharmaceutical science].

The separation of organic compounds has been carried out using the method of distillation and recrystallization since the 17th century.1st separation technology innovation (1950s to 1960s). After World War II, the science of separating organic compounds evolved to the use of paper or column chromatography. 2nd separation technology innovation (1960s to 1980s). In the 1960s, thin-layer chromatograpy (TLC) was developed. TLC is a convenient analytical technique for organic compounds. Separation methods for organic compounds using column chromatography and preparative TLC were carried out as practical applications. Gas chromatography (GC) was also introduced in the 1960s. GC is a useful analytical method for a mixture of various volatile organic compounds. Many GC instruments with new kinds of sensors were developed. Gas chromatography of nonbenzenoid organometallic compounds and metal complexes was successfully conducted by the author. 3rd separation technology innovation (1980s to 1990s). In the 1980s, high-performance liquid-chromatography (HPLC) was developed. HPLC analytical methods were useful for various kinds of organic compounds. In the 1990s, LC-MS and LC-NMR instruments were introduced for biomedical products. 4th separation technology innovation (1990s to present). Several new ionization methods for mass-spectrometry (electrospray, matrix-aided lazer desorption ionization, etc) are applied for proteins and biomedical products. Several new separation technologies (supercritical field chromatography, capillary electrophoresis, field-flow fractionization, etc.) are now being developed.

History, 20th Century↗

PubMed2005

An experimental model for the determination of immunomodulating effects by volatile compounds.

An in vitro exposure system was developed to enable simultaneous exposure of primary cells or cell lines to defined concentrations of volatile organic compounds (VOC) without the necessity of a constant-flow exposure system. Toluene was used as model VOC and administered via the gas phase. CD3/CD28-stimulated human peripheral blood mononuclear cells (PBMC) were used as indicator cells. Vitality/proliferation of PBMC was tested using the MTT assay and their functional reactivity using cytokine ELISA for interferon-gamma (IFN-gamma), interleukin-4 (IL-4), IL-13, and tumor-necrosis-factor-alpha (TNF-alpha). Chemical analysis using headspace gas chromatography confirmed that this new method guaranties reproducible VOC exposure (R2 = 0.995 for the correlation between external toluene concentration and toluene in the cell culture). While cytotoxic effects were not observed, dose-dependent toluene effects on functional reactivity of PBMC were found. The secretion of IFN-gamma, IL-4, and IL-13 was inhibited at concentrations of 72.5 g/m3 and above, whereas the TNF-alpha production was increased. Since the presented in vitro model ensures toluene exposure in concentrations comparable to the real situation, and allows the investigation of dose-dependent immunomodulatory toluene effects in concentrations without cytotoxicity, this method first described here is introduced as useful tool in analysis of VOC-triggered effects on immune cells.

Cell Proliferation↗

PubMed2003

Computation of log BB values for compounds transported through carrier-mediated mechanisms using in vitro permeability data from brain microvessel endothelial cell (BMEC) monolayers.

PURPOSE: To explore the possibility of determining in vivo log BB values (the logarithm value of brain to plasma concentration ratio) from in vitro permeability data measured in brain microvessel endothelial cell (BMEC) monolayers. METHODS: An equilibrium mathematical model was developed: log BB = log(Ca/Cb) + log Kbr:pl, where Cb and Ca are the drug concentrations at equilibrium in the basolateral (B) and apical (A) sides of BMECs in an A-to-B directional diffusion system and Kbr:pl is the brain-plasma partition coefficient. With this model, murine log BB values were calculated for 24 pharmaceutical compounds, mostly Pgp substrates. RESULTS: Calculated log BB values correlated well to experimental values (r2 = 0.854, slope = 0.907 +/- 0.080), demonstrating that the model could reasonably predict brain penetration for compounds that are involved in carrier-mediated transport mechanisms. For a second data set that included volatile organic compounds (log BB = log Kbr:pl), log Kbr:pl values were also shown to correlate well with their respective experimental log BB values (r2 = 0.876, slope = 0.973 +/- 0.082), demonstrating that log Kbr:pl is an excellent descriptor for log BB when a compound penetrates the blood-brain barrier by passive diffusion only. CONCLUSION: The equilibrium model demonstrated a reasonable ability to compute in vivo log BB values, regardless of the involvement or mechanisms of carrier-mediated transport.

Animals↗

PubMedDate not supplied

Building-related illness and employee lost time following application of hot asphalt roof: a call for prevention.

Industrial hygiene sampling within an office building during and following a roof renovation revealed low-level exposure to high-boiling organic compounds, associated with complaints of eye and upper respiratory tract irritation among building occupants. Health complaints continued substantially beyond the time frame of the renovation completion, despite a lack of objective industrial hygiene findings for volatile organic compounds (VOCs) and microbiological contamination, and a lack of consistent medical findings among employees evaluated by an occupational physician. An analysis of employee attendance records suggests lost attendance and reduced productivity costs. Preventive strategies include proper planning and scheduling of building renovations to prevent employee exposure to asphalt roof emissions.

Adult↗

PubMed1998

Parts-per-trillion determination of styrene in yoghurt by purge-and-trap gas chromatography with mass spectrometry detection.

Headspace sampling methods prior to capillary gas chromatography have been widely used for the determination of volatile compounds present in very different kinds of samples. This paper describes an automated and rapid system to determine volatiles from yoghurt. Thirty-five volatile organic compounds (VOCs) were identified in polystyrene cups used for yoghurt packaging and 42 VOCs from yoghurt samples. Quantitation of styrene in several samples from the Spanish retail market was carried out.

Chromatography, Gas↗

PubMed2005

A process to prepare a synthetic filter material containing nutrients for biofiltration.

In this study, an optimal process to prepare a synthetic filter material (poly(vinyl alcohol) (PVA)/peat/KNO(3) composite bead) containing nutrients was developed for biofiltration. The optimal preparing condition was that each of the peat and PVA aqueous solutions contains 6.4 g KNO(3) and the nitrogen content in the boric and phosphate aqueous solutions must retain higher than 3.94 and 1.52 g N/l, respectively. The equilibrium amount of water-soluble nitrogen dissolved out of the prepared composite bead was between 7.95 and 8.21mg N/g dry solid. The path of water-soluble nitrogen dissolving out of the A-type bead was the water-soluble nitrogen dispersed in the peat phase initially diffused into the outer PVA phase and then it diffused out of the bead surface. And the path of water-soluble nitrogen dissolving out of the H-type bead was the water-soluble nitrogen dispersed in both the peat and PVA phases simultaneously diffused into the outer PVA phase and out of the bead surface, respectively. The microbial growth rate k(g) of the H-type composite bead was higher than that of the A-type composite bead approximately 1.09-1.58 times, and its value was between 0.100 and 0.417 day(-1) as the composite bead was immersed in 0-0.896 M KNO(3) solution. The maximum value of k(g) appeared at the composite bead immersed in 0.384 M KNO(3) solution and was higher than that of the compost by a factor approximately 1.49. The percentage of removed volatile organic compounds (VOCs) remained at more than 98% during the biofilter operating 230 days as the composite bead was immersed in KNO(3) aqueous solution before packing. This composite bed was without the further addition of nutrients during this operating period. It was proved that this composite bead was superior to the compost as a filter material.

Air Pollutants↗

PubMed2002

Structural investigation of catalyst deactivation of Pt/SDB for catalytic oxidation of VOC-containing wastewater.

The stability of styrene-divinyl benzene copolymer (SDB)-supported Pt (Pt/SDB) catalysts for destruction of volatile-organic-compound (VOC) in wastewater was examined. The test reaction was wet oxidation of water-containing aliphatic alcohol and formaldehyde at 140 degrees C and 90 psig for 40 h. The catalytic performance tests indicated that activity of the Pt/SDB catalysts could be maintained for VOC concentration of 3 wt.%, whereas the catalysts deactivated rapidly for 10 wt.% VOC containing wastewater. In order to investigate the nature of catalyst deactivation, extended X-ray absorption fine structure (EXAFS) and X-ray absorption near edge (XANES) spectroscopy were used to characterize the fresh and used catalysts. After the reaction, there is no oxidation of Pt clusters observed in EXAFS and XANES spectroscopy suggesting that the oxidation reaction takes places via the adsorbed oxygen. The spectroscopy results further indicated that deactivation of the catalysts were mainly caused by the increase of Pd particle size. After the reaction, the Pt-Pt coordination number has no significant change for the 3 wt.% wastewater whereas increase from 5.6 to 6.2 for 10 wt.% wastewater. Combined with the fact that the catalysts fractured during the reactions, we suggested that Pt agglomeration was mainly caused by thermal migration of the metal clusters.

Catalysis↗

PubMed1995

Effect of crop development on biogenic emissions from plant populations grown in closed plant growth chambers.

The Biomass Production Chamber at John F. Kennedy Space Center is a closed plant growth chamber facility that can be used to monitor the level of biogenic emissions from large populations of plants throughout their entire growth cycle. The head space atmosphere of a 26-day-old lettuce (Lactuca sativa cv. Waldmann's Green) stand was repeatedly sampled and emissions identified and quantified using GC-mass spectrometry. Concentrations of dimethyl sulphide, carbon disulphide, alpha-pinene, furan and 2-methylfuran were not significantly different throughout the day; whereas, isoprene showed significant differences in concentration between samples collected in light and dark periods. Volatile organic compounds from the atmosphere of wheat (Triticum aestivum cv. Yecora Rojo) were analysed and quantified from planting to maturity. Volatile plant-derived compounds included 1-butanol, 2-ethyl-1-hexanol, nonanal, benzaldehyde, tetramethylurea, tetramethylthiourea, 2-methylfuran and 3-methylfuran. Concentrations of volatiles were determined during seedling establishment, vegetative growth, anthesis, grain fill and senescence and found to vary depending on the developmental stage. Atmospheric concentrations of benzaldehyde and nonanal were highest during anthesis, 2-methylfuran and 3-methylfuran concentrations were greatest during grain fill, and the concentration of the tetramethylurea peaked during senescence.

Biomass↗

PubMed2002

C6-Green leaf volatiles trigger local and systemic VOC emissions in tomato.

In response to insect feeding, tomato plants (Lycopersicon esculentum) release elevated levels of volatile organic compounds; that is, monoterpenes and sesquiterpenes are released both locally and systemically with wounding while C(6) green leaf volatiles are released only from damaged leaves. With the exogenous application (100 nmol) of the C(6)-tomato-volatile (E)-2-hexenal, an increase in the release of local and systemic terpenes was observed, while an equimolar amount of methyl jasmonate triggered only local emissions of terpenes. Labeling studies with 13CO(2) showed that de novo synthesis was not required for monoterpene or sesquiterpene release immediately following chemical treatment or insect feeding. Comparative measurements were made between aldehyde doses applied to the plant and levels naturally released from leaves with insect damage.

Animals↗

PubMed2003

Solid-phase microextraction of volatile compounds from the chopped leaves of three species of Eucalyptus.

Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography and ion-trap mass spectrometry has been used to identify biogenic volatile organic compounds present in the headspace of chopped leaves of Eucalyptus (E.) dunnii, E. citriodora, and E. saligna. A simple HS-SPME method entailing 30 min of extraction at 30 degrees C was developed for this purpose. Thirty compounds were identified in the headspace of 60 juvenile chopped Eucalyptus leaves, and another 30 were tentatively identified. The presence of compounds such as (E)-4,8-dimethyl-1,3,7-nonatriene (DMNT), (E,E)-4,8,12-trimethyl-1,3,7,11-tridecatetraene (TMNT), (E,E)-alpha-farnesene, (E,E,E)-3,7,11,15-tetramethyl-1,3,6,10,14-hexadecapentaene (TMHP), beta-caryophyllene, alpha-humulene, germacrene D, and beta-cubebene in the headspace of the leaves but not in the essential oils from the same Eucalyptus trees and information about the infochemical roles of some of these compounds in other living plant systems suggest they might play a bioactive role in Eucalyptus leaves.

Eucalyptus↗

PubMed2001

Chemical composition of some traditional herbal drug preparations: essential oil and aromatic water of costmary (Balsamita suaveolens Pers.).

The compositions of the essential oil and the aromatic water of costmary (Balsamita suaveolens Pers.) cultivated in Tuscany were investigated. They represent the main ingredients of some traditional preparations sold commercially. The essential oil as such and the n-hexane extract of the aromatic water were analyzed by GC and GC-MS. Both samples were found to be rich in monoterpenes. Eighty-five compounds were identified, accounting for 95.1 and 95.4% of the essential oil and n-hexane extract of aromatic water, respectively. Carvone was the main compound (43.5% in the essential oil and 74.9% in the n-hexane extract of aromatic water). In addition, solid phase microextraction was used to sample the volatile organic compounds emitted from the fresh plant and from the aromatic water, and carvone was again the main component, amounting to 46.2 and 41.3%, respectively.

Antineoplastic Agents, Phytogenic↗

PubMed2000

Carbon isotope effects resulting from equilibrium sorption of dissolved VOCs.

To accurately interpret isotopic data obtained for volatile organic compounds (VOCs) dissolved in groundwater systems, the isotopic effects of subsurface processes must be understood. Previous work has demonstrated that volatilization and dissolution of BTEX and chlorinated ethene compounds are not significantly isotopically fractionating. This study characterized the carbon isotopic effects of equilibrium sorption of perchloroethylene, trichloroethylene, benzene, and toluene to both graphite and activated carbon directly in batch experiments over a range of 10-90% sorption. Results demonstrate that, over this range, equilibrium sorption of these VOCs to graphite and activated carbon does not result in significant carbon isotopic fractionation within the +/-0.5% accuracy and reproducibility associated with compound-specific isotope analysis. This implies that the isotopic values of dissolved VOCs will not be significantly affected by equilibrium sorption in the subsurface. Therefore, isotopic analysis has potential to be used in the field to differentiate between mass losses due to isotopically fractionating processes such as biodegradation versus mass loss due to nondegradative processes.

Journal Article↗

PubMed2003

A 50% n-octylmethyl, 50% diphenyl-polysiloxane as stationary phase with unique selectivity for gas chromatography.

An n-octylmethyl, diphenyl-polysiloxane called SOP-50-Octyl was prepared by a condensation reaction of bis(dimethylamino) n-octylmethylsilane with diphenylsilanediol. The resulting copolymer was a gum with high molecular weight and was obtained with a yield of 80%. 1H and 29Si NMR spectroscopy revealed that the copolymer was a 52% octylmethyl, 48% diphenyl-polysiloxane with random microstructure. Small cyclic impurities could be almost quantitatively removed via a purification step. SOP-50-Octyl was used as stationary phase for the preparation of wall coated open tubular fused silica capillary columns for gas-liquid chromatography. The capillary columns exhibited high separation efficiency and high inertness. The stationary phase offered a unique selectivity due to its unique composition. The Rohrschneider-McReynolds constants indicated a low overall polarity in spite of the high phenyl content, as the polarity was distinctly decreased by the octyl substituent. Furthermore, the octyl substituent was responsible for a high column bleed, reducing the maximum allowable operating temperature to 280 degrees C. The elution temperatures of apolar compounds were increased due to increased interaction of the octyl substituent with the analytes. Some applications with volatile and semi-volatile organic compounds illustrate that SOP-50-Octyl is an excellent choice for confirmational analyses.

Chromatography, Gas↗

PubMed2006

Dynamics of the enhanced emissions of monoterpenes and methyl salicylate, and decreased uptake of formaldehyde, by Quercus ilex leaves after application of jasmonic acid.

Jasmonic acid (JA) is a signalling compound with a key role in both stress and development in plants, and is reported to elicit the emission of volatile organic compounds (VOCs). Here we studied the dynamics of such emissions and the linkage with photosynthetic rates and stomatal conductance. We sprayed JA on leaves of the Mediterranean tree species Quercus ilex and measured the photosynthetic rates, stomatal conductances, and emissions and uptake of VOCs using proton transfer reaction mass spectrometry and gas chromatography after a dark-light transition. Jasmonic acid treatment delayed the induction of photosynthesis and stomatal conductance by approx. 20 min, and decreased them 24 h after spraying. Indications were found of both stomatal and nonstomatal limitations of photosynthesis. Monoterpene emissions were enhanced (20-30%) after JA spraying. Jasmonic acid also increased methyl salicylate (MeSa) emissions (more than twofold) 1 h after treatment, although after 24 h this effect had disappeared. Formaldehyde foliar uptake decreased significantly 24 h after JA treatment. Both biotic and abiotic stresses can thus affect plant VOC emissions through their strong impact on JA levels. Jasmonic acid-mediated increases in monoterpene and MeSa emissions might have a protective role when confronting biotic and abiotic stresses.

Carbon Dioxide↗