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1.
J Hazard Mater ; 453: 131446, 2023 07 05.
Artigo em Inglês | MEDLINE | ID: mdl-37088025

RESUMO

Bis (2-chloro-1-methylethyl) ether (DCIP), one U.S. Environmental Protection Agency priority pollutant, could pose health and/or odor risk in water environment. In this study, odor characteristics, occurrence and source of DCIP in drinking waters of China were investigated based on sensory analysis and a nation-wide investigation covering 140 drinking water treatment plants. Then multi-risk integrated health and aesthetic aspects through oral and inhalation (showering) exposure by drinking water were first estimated. Sensory evaluation showed DCIP exhibited "solvent-like" odor with thresholds of 34.8 ng/L in air and 142.0 ng/L in water. DCIP was detected at comparable concentrations in raw and finished waters (<1280 ng/L) and was by-product from industrial production of epichlorohydrin/propylene oxide. Lifetime Average Daily Dose through oral exposure was 0-36.65 ng/day/kg, corresponding to odor activity values of 0-8.4 and hazard quotients of far < 1, indicating drinking tap water might cause odor issues rather than significant health hazard. The proportion of sensitive population to DCIP's odor was 6.1%. In contrast, residents rarely detect DCIP's odor by inhalation. The presence in drinking water as industrial by-product, poor removal using conventional water treatment and potential to be T&O issues, indicates urgent demand for pollutant source control to protect DCIP from entering source waters.


Assuntos
Água Potável , Poluentes Ambientais , Poluentes Químicos da Água , Água Potável/análise , Éter/análise , Solventes , Poluentes Químicos da Água/análise , Éteres , Etil-Éteres , Poluentes Ambientais/análise , Medição de Risco , China , Monitoramento Ambiental
2.
Arch Microbiol ; 204(8): 531, 2022 Jul 29.
Artigo em Inglês | MEDLINE | ID: mdl-35904606

RESUMO

There is an urgent need to develop natural antimicrobials for the control of rapidly mutating drug-resistant bacteria and poultry viruses. Five extracts were prepared using diethyl ether, ethyl acetate, methanol, 1-butanol and n-hexane from abdominal fats of Varanus griseus locally known as Indian desert monitor. Antibacterial, antioxidant and antiviral activities from oil extracts were done through disc diffusion method, stable 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging assay and in ovo antiviral assay, respectively. The gas chromatography mass spectrometry (GC-MS) analyses were used to determine principal active compounds and chemical profile of each oil extract. n-Hexane extract showed clear zones of inhibition (ZOI) against Staphylococcus aureus, Escherichia coli and Klebsiella pneumoniae (12 ± 0.5 mm, 9 ± 0.5 mm, and 9 ± 0.5 mm) while diethyl ether extract exhibited significant antibacterial activity (11 ± 0.5 mm) against Proteus vulgaris only. In case of drug-resistant strains, methanol extract was active (6 ± 0.5 mm) against Staphylococcus aureus, whereas n-hexane extract has shown ZOI 11 ± 0.5 mm against P. aeruginosa. Range of percentage scavenging activity of V. griseus oil extracts from DPPH free radical assay was 34.9-70.7%. For antiviral potential, growth of new castle disease virus (NDV) was effectively inhibited by all five extracts (HA titer = 0-4). The highest antiviral activity against avian influenza virus (H9N2) was observed from methanol, diethyl ether and 1-Butanol oil extracts with HA titers of 2, 2 and 0, respectively. Methanol, diethyl ether, 1-butanol and n-hexane oil extracts produced best hemagglutination assay (HA) titer values (0, 0, 4 and 0) against infectious bronchitis virus (IBV). Ethyl acetate and 1-Butanol extract exhibited good antiviral potential against infectious bursal disease virus (IBDV) with indirect hemagglutination assay (IHA) titers of 8 and 4, respectively. Main classes of identified compounds through gas chromatography were aldehydes, fatty acids, phenols and esters. GC-MS identified 11 bioactive compounds in V. griseus oil extracts. It is summarized that V. griseus oil has strong antioxidant activity and good antimicrobial potential because of its bioactive compounds.


Assuntos
Anti-Infecciosos , Vírus da Influenza A Subtipo H9N2 , 1-Butanol/análise , Animais , Antibacterianos/química , Anti-Infecciosos/farmacologia , Antioxidantes/análise , Antivirais/farmacologia , Éter/análise , Radicais Livres/análise , Cromatografia Gasosa-Espectrometria de Massas , Metanol , Testes de Sensibilidade Microbiana , Extratos Vegetais/química , Extratos Vegetais/farmacologia
3.
J Anim Sci ; 100(9)2022 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-35894938

RESUMO

Previous research demonstrated that a fixed value of 0.2433 (SE = 0.0134) Mcal of CH4/kg of dry matter intake (DMI) could be used to predict CH4 production with accuracy and precision on par with similar equations in the literature. Slope bias was substantially less for the fixed-coefficient equation than noted for the other DMI- or gross energy intake (GEI)-based equations, but mean bias was substantially greater, presumably reflecting the failure of the fixed-coefficient approach to account for dietary factors that affect CH4 production. In this article, we report on the use of the dietary ratio of concentrations of starch to neutral detergent fiber (NDF) and dietary ether extract (EE) concentration to improve the accuracy and precision of the fixed-coefficient equation. The same development data set used to create the fixed-coefficient equation was used in the present study, which included 134 treatment means from 34 respiration calorimetry studies. Based on stepwise regression with dietary NDF, starch, crude protein, EE, and the starch:NDF ratio as possible dependent variables, the starch:NDF ratio and EE were the only dietary variables selected (P ≤ 0.15). The study-adjusted relationship with the starch:NDF ratio (r2 = 0.673; root mean square error [RMSE] = 0.0327) was: Mcal of CH4/kg of DMI = 0.2883 - 0.03474 × starch:NDF; whereas the relationship with a model that included both starch:NDF ratio and dietary EE (r2 = 0.738; RMSE = 0.0315) was: Mcal of CH4/kg of DMI = 0.3227 - 0.0334 × starch:NDF - 0.00868 × % EE. A previously published independent data set with 129 treatment means from 30 respiration calorimetry studies was used to evaluate these two equations, along with two additional equations in which g/d of CH4 was predicted directly from DMI, starch:NDF ratio, and/or dietary EE. The two Mcal of CH4/kg of DMI equations had superior fit statistics to the previously published 0.2433 Mcal of CH4/kg of DMI equation, with a substantial decrease in mean bias and improved concordance correlation coefficients. Moreover, the Mcal of CH4/kg of DMI equations resulted in improved fit relative to direct prediction of g/d of CH4 from DMI, the starch:NDF ratio, and % EE. Based on these results, further evaluation of the dietary ratio of starch-to-NDF concentrations and EE concentration to predict methane production per unit DMI in beef cattle is warranted.


Accurate and precise equations to predict enteric methane production are an important tool as the beef industry works to mitigate greenhouse gas emissions. We predicted the megacalories of methane per unit of dry matter intake using data from growing and finishing beef and dairy steers and heifers. The predicted value was then multiplied by dry matter intake to estimate methane production. The most important predictor variables were the ratio of dietary starch to neutral detergent fiber concentrations and dietary ether extract concentration. When tested with an independent data set, predicting methane per unit dry matter intake from the ratio of starch to neutral detergent fiber, with or without the addition of dietary ether extract as a predictor variable, yielded better fits to the independent data set than equations in which the daily production of methane was predicted directly from dry matter intake, the ratio of starch to neutral detergent fiber, and/or dietary ether extract. Predictions could potentially be further refined by adjusting the starch component of the ratio for degradability in the rumen (e.g., degree of gelatinization or processing) and the neutral detergent fiber content for the contributions from roughage vs. grains and grain byproducts.


Assuntos
Metano , Amido , Animais , Bovinos , Detergentes/análise , Dieta/veterinária , Fibras na Dieta/metabolismo , Éter/análise , Feminino , Lactação , Leite/metabolismo , Extratos Vegetais , Amido/metabolismo
4.
Curr Biol ; 30(19): 3775-3787.e7, 2020 10 05.
Artigo em Inglês | MEDLINE | ID: mdl-32857977

RESUMO

Sphingolipids play important roles in physiology and cell biology, but a systematic examination of their functions is lacking. We performed a genome-wide CRISPRi screen in sphingolipid-depleted human cells and identified hypersensitive mutants in genes of membrane trafficking and lipid biosynthesis, including ether lipid synthesis. Systematic lipidomic analysis showed a coordinate regulation of ether lipids with sphingolipids, suggesting an adaptation and functional compensation. Biophysical experiments on model membranes show common properties of these structurally diverse lipids that also share a known function as glycosylphosphatidylinositol (GPI) anchors in different kingdoms of life. Molecular dynamics simulations show a selective enrichment of ether phosphatidylcholine around p24 proteins, which are receptors for the export of GPI-anchored proteins and have been shown to bind a specific sphingomyelin species. Our results support a model of convergent evolution of proteins and lipids, based on their physico-chemical properties, to regulate GPI-anchored protein transport and maintain homeostasis in the early secretory pathway.


Assuntos
Éteres Fosfolipídicos/metabolismo , Via Secretória/fisiologia , Esfingolipídeos/metabolismo , Animais , Linhagem Celular , Membrana Celular/metabolismo , Retículo Endoplasmático/metabolismo , Éter/análise , Éter/metabolismo , Glicosilfosfatidilinositóis/análise , Glicosilfosfatidilinositóis/metabolismo , Humanos , Lipídeos/biossíntese , Proteínas de Membrana/metabolismo , Proteínas de Membrana Transportadoras/metabolismo , Camundongos , Transporte Proteico/fisiologia , Esfingolipídeos/fisiologia
5.
Environ Sci Pollut Res Int ; 27(5): 5085-5096, 2020 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-31848954

RESUMO

2,2',4,4'-Tretrabromodiphenyl ether (BDE47) is known as a typical polybrominated diphenyl ethers (PBDEs) due to its high environmental abundance, ecological toxicity, and bioaccumulation. In this study, the influences of three typical surfactants (CTAB, SDS, and TX-100) on BDE47 solubilization and degradation by the polyanionic cellulose-stabilized Pd/Fe (PAC-Pd/Fe) nanoparticles were investigated. The results showed that BDE47 solubilities increased linearly when surfactant concentrations were above their critical micelle concentrations (CMCs), and the solubilization capacities of surfactants for BDE47 followed the order of TX-100 > CTAB > SDS. The appropriate dosages of surfactants were favorable for BDE47 degradation due to enhancing solubilization and accelerating mass transfer, while excessive surfactants inhibited BDE47 degradation due to excessive and thicker micelles formed, but still higher than no surfactant. The influences of various factors (PAC-Pd/Fe nanoparticle dosage, solution pH, and temperature) on BDE47 degradation in TX-100 solution were also tested. The results showed that BDE47 degradation followed the pseudo first-order kinetics model. The degradation rates of BDE47 increased as PAC-Pd/Fe nanoparticle dosage and temperature increased. Weak acidic condition (pH 5.5) was favorable for BDE47 degradation with 96.8% BDE47 was removed within 7.5 min, while alkaline condition (9.0) was not conducive to the degradation of BDE47. The degradation of BDE47 by PAC-Pd/Fe nanoparticles was a catalytic reductive debromination process via active H-species attack, wherein the sequential debromination was the dominant reaction. This study suggests that in the presence of moderate surfactant, PAC-Pd/Fe nanoparticles may be potentially employed to eliminate BDE47 in contaminated water.


Assuntos
Éter , Nanopartículas , Aminação , Éter/análise , Éteres Difenil Halogenados/química , Ferro/química , Tensoativos
6.
Chem Biodivers ; 16(7): e1900153, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-31063673

RESUMO

Some carnation species (Dianthus spp., Caryophyllaceae) exhibit a strong resistance to drought stress that is connected with the increased surface wax formation. Wax composition is unknown for the majority of Dianthus spp. Herein, mass spectral and gas chromatographic data, in combination with synthesis and chemical transformations (transesterification and synthesis of dimethyl disulfide adducts), enabled the identification of 151 constituents of diethyl-ether washings of fresh flowers of Dianthus cruentus Griseb. from Serbia. The flower wax contained, along with the dominant ubiquitous long-chain n-alkanes, homologous series of n- and branched (iso- and anteiso-) long-chain hexyl alkanoates/alkenoates and alkyl/alkenyl benzoates. The branching position in the mentioned hexyl esters was probed by synthesis of esters of three isomeric hexanols that were spectrally characterized (1 H- and 13 C-NMR, IR, MS). The washings also contained long-chain (Z)- and (E)-alkenes (C23 -C35 ) with several different double bond regiochemistries. Fifty-five of these constituents (eight hexyl esters, two benzoates, and forty-five alkenes) were detected for the first time in Plantae, while ten of these represent completely new compounds. The rare occurrence of these wax constituents makes them possible chemotaxonomic markers of this particular Dianthus sp.


Assuntos
Caryophyllaceae/química , Éter/análise , Flores/química , Alcenos/análise , Benzoatos/análise , Cromatografia Gasosa-Espectrometria de Massas , Estrutura Molecular
7.
PLoS One ; 13(6): e0198913, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-29912920

RESUMO

Analytical devices that combine sensitive biological component with a physicochemical detector hold a great potential for various applications, e.g., environmental monitoring, food analysis or medical diagnostics. Continuous efforts to develop inexpensive sensitive biodevices for detecting target substances typically focus on the design of biorecognition elements and their physical implementation, while the methods for processing signals generated by such devices have received far less attention. Here, we present fundamental considerations related to signal processing in biosensor design and investigate how undemanding signal treatment facilitates calibration and operation of enzyme-based biodevices. Our signal treatment approach was thoroughly validated with two model systems: (i) a biodevice for detecting chemical warfare agents and environmental pollutants based on the activity of haloalkane dehalogenase, with the sensitive range for bis(2-chloroethyl) ether of 0.01-0.8 mM and (ii) a biodevice for detecting hazardous pesticides based on the activity of γ-hexachlorocyclohexane dehydrochlorinase with the sensitive range for γ-hexachlorocyclohexane of 0.01-0.3 mM. We demonstrate that the advanced signal processing based on curve fitting enables precise quantification of parameters important for sensitive operation of enzyme-based biodevices, including: (i) automated exclusion of signal regions with substantial noise, (ii) derivation of calibration curves with significantly reduced error, (iii) shortening of the detection time, and (iv) reliable extrapolation of the signal to the initial conditions. The presented simple signal curve fitting supports rational design of optimal system setup by explicit and flexible quantification of its properties and will find a broad use in the development of sensitive and robust biodevices.


Assuntos
Técnicas Biossensoriais/métodos , Enzimas/metabolismo , Processamento de Sinais Assistido por Computador , Calibragem , Substâncias para a Guerra Química/análise , Poluentes Ambientais/análise , Éter/análogos & derivados , Éter/análise , Hexanos/análise , Hidrocarbonetos Clorados/análise , Hidrolases/metabolismo , Liases/metabolismo , Sensibilidade e Especificidade
8.
An. acad. bras. ciênc ; 89(2): 1295-1303, Apr.-June 2017. tab
Artigo em Inglês | LILACS | ID: biblio-886692

RESUMO

ABSTRACT The objective of this study was to compare the estimates of ether extract (EE) contents obtained by the Randall method and by the high-temperature method of the American Oil Chemist's Society (AOCS; Am 5-04) in forages (n = 20) and cattle feces (n = 15). The EE contents were quantified by using the Randall extraction or AOCS method and XT4 filter bags or cartridges made of qualitative filter paper (80 g/m²) as containers for the samples. It was also evaluated the loss of particles, and concentration of residual chlorophyll after extraction and the recovery of protein and minerals in the material subjected to extraction. Significant interaction was observed between extraction method and material for EE contents. The EE estimates using the AOCS method were higher, mainly in forages. No loss of particles was observed with different containers. The chlorophyll contents in the residues of cattle feces were not affected by the extraction method; however, residual chlorophyll was lower using the AOCS method in forages. There was complete recovery of the protein and ash after extraction. The results suggest that AOCS method produces higher estimates of EE contents in forages and cattle feces, possibly by providing greater extraction of non-fatty EE.


Assuntos
Animais , Técnicas de Química Analítica/métodos , Éter/análise , Éter/química , Fezes/química , Poaceae/química , Ração Animal/análise , Bovinos , Reprodutibilidade dos Testes , Análise de Alimentos/métodos , Temperatura Alta
9.
An Acad Bras Cienc ; 89(2): 1295-1303, 2017.
Artigo em Inglês | MEDLINE | ID: mdl-28489203

RESUMO

The objective of this study was to compare the estimates of ether extract (EE) contents obtained by the Randall method and by the high-temperature method of the American Oil Chemist's Society (AOCS; Am 5-04) in forages (n = 20) and cattle feces (n = 15). The EE contents were quantified by using the Randall extraction or AOCS method and XT4 filter bags or cartridges made of qualitative filter paper (80 g/m²) as containers for the samples. It was also evaluated the loss of particles, and concentration of residual chlorophyll after extraction and the recovery of protein and minerals in the material subjected to extraction. Significant interaction was observed between extraction method and material for EE contents. The EE estimates using the AOCS method were higher, mainly in forages. No loss of particles was observed with different containers. The chlorophyll contents in the residues of cattle feces were not affected by the extraction method; however, residual chlorophyll was lower using the AOCS method in forages. There was complete recovery of the protein and ash after extraction. The results suggest that AOCS method produces higher estimates of EE contents in forages and cattle feces, possibly by providing greater extraction of non-fatty EE.


Assuntos
Ração Animal/análise , Técnicas de Química Analítica/métodos , Éter/análise , Éter/química , Fezes/química , Poaceae/química , Animais , Bovinos , Análise de Alimentos/métodos , Temperatura Alta , Reprodutibilidade dos Testes
10.
Sci Rep ; 6: 39270, 2016 12 20.
Artigo em Inglês | MEDLINE | ID: mdl-27995977

RESUMO

3-Methyldiphenylether (MDE) is an important alkyl-substituted diphenyl ether compound that is widely used as an intermediate in the synthesis of pyrethroid insecticides. An efficient MDE-degrading strain QY7-2, identified as Hydrogenophaga atypical, was isolated from activated sludge for the first time. Strain QY7-2 can utilize MDE as the sole carbon and energy source and completely mineralize MDE. The degradation pathway of MDE was proposed in the strain through metabolites identification. A gene cluster involving in methy-oxidation of MDE was cloned from QY7-2 and expressed in Escherichia coli BL21 (DE3), and the products were purified by SDS-PAGE. The specific activities of the recombinant enzymes MdeAB, MdeC and MdeD were 113.8 ± 3.5, 274.5 ± 6.2 and 673.4 ± 8.7 nmol min-1 mg-1, respectively. These results provide the biochemical and genetic foundation of microbial degradation pathway of MDE and benefit the bioremediation of MDE-contaminated environments.


Assuntos
Subfamília D de Transportador de Cassetes de Ligação de ATP/metabolismo , Clonagem Molecular , Comamonadaceae/metabolismo , Éter/metabolismo , Subfamília D de Transportador de Cassetes de Ligação de ATP/genética , Proteínas de Bactérias/genética , Proteínas de Bactérias/metabolismo , Biodegradação Ambiental , Cromatografia Líquida de Alta Pressão , Escherichia coli/metabolismo , Éter/análise , Éter/química , Cinética , Mutagênese , Espectrometria de Massas em Tandem
11.
J Chromatogr A ; 1468: 136-142, 2016 Oct 14.
Artigo em Inglês | MEDLINE | ID: mdl-27658381

RESUMO

A Porous Graphitic Carbon (PGC) column was evaluated for the analysis of poly(phenylene ether) (PPE). This column appears particularly well-suited for the separation of this polymer. Conditions for the elution of PPE either in adsorption mode with chloroform or size exclusion with 1,2,4-trichlorobenzene (TCB) as eluent were established. Elution of homologous species is obtained in chloroform that follows Martin's rule. A separation based on a gradient consisting of a sequence of non-solvent (acetonitrile), solvent/adsorli (chloroform) provided the highest peak capacity. In TCB, it is possible to obtain rapid size-based separation: with a flow rate of 0.7ml/min, the run time is less than two minutes for a series of polystyrene standards. The PGC column performs remarkably well in this mode and may be a viable solution when a short analysis time is critical such as in a combinatorial laboratory or in a two-dimensional chromatograph. In addition to its value as a sorbent for polymer separation, this column also deserves the attention of the materials engineer. Indeed, the PGC sorbent can be used as a model to probe the interaction between polymers and graphitic fillers such as carbon nanotubes or graphite nanosheets.


Assuntos
Técnicas de Química Analítica/métodos , Cromatografia Líquida , Éter/análise , Grafite/química , Acetonitrilas/química , Adsorção , Técnicas de Química Analítica/instrumentação , Clorobenzenos/química , Clorofórmio/química , Éter/química , Éteres/química , Microscopia Eletrônica de Varredura , Polímeros/química , Porosidade , Solventes/química
12.
Biotechnol Bioeng ; 113(9): 1853-61, 2016 09.
Artigo em Inglês | MEDLINE | ID: mdl-26915048

RESUMO

We constructed an enzymatic network composed of three different enzymes for the synthesis of valuable ether amines. The enzymatic reactions are interconnected to catalyze the oxidation and subsequent transamination of the substrate and to provide cofactor recycling. This allows production of the desired ether amines from the corresponding ether alcohols with inorganic ammonium as the only additional substrate. To examine conversion, individual and overall reaction equilibria were established. Using these data, it was found that the experimentally observed conversions of up to 60% observed for reactions containing 10 mM alcohol and up to 280 mM ammonia corresponded well to predicted conversions. The results indicate that efficient amination can be driven by high concentrations of ammonia and may require improving enzyme robustness for scale-up. Biotechnol. Bioeng. 2016;113: 1853-1861. © 2016 Wiley Periodicals, Inc.


Assuntos
Álcool Desidrogenase/metabolismo , Álcoois/metabolismo , Aminas/metabolismo , Éter/metabolismo , Transaminases/metabolismo , Álcoois/química , Aminas/análise , Aminas/química , Bactérias/enzimologia , Bactérias/genética , Proteínas de Bactérias/metabolismo , Biocatálise , Éter/análise , Éter/química
13.
Environ Sci Technol ; 49(21): 12758-65, 2015 Nov 03.
Artigo em Inglês | MEDLINE | ID: mdl-26444952

RESUMO

Bound-residue formation is a major dissipation process of most organic xenobiotics in soil. However, both the formation and nature of bound residues of tetrabromobisphenol A (TBBPA) in soil are unclear. Using a 14C-tracer, we studied the fate of TBBPA in an oxic soil during 143 days of incubation. TBBPA dissipated with a half-life of 14.7 days; at the end of incubation, 19.6% mineralized and 66.5% formed bound residues. Eight extractable metabolites were detected, including TBBPA methyl ethers, single-ring bromophenols, and their methyl ethers. Bound residues (mostly bound to humin) rapidly formed during the first 35 days. The amount of those humin-bound residues then quickly decreased, whereas total bound residues decreased slowly. By contrast, residues bound to humic acids and fulvic acids increased continuously until a plateau was reached. Ester- and ether-linked residues accounted for 9.6-27.0% of total bound residues during the incubation, with ester linkages being predominant. Residues bound via ester linkages consisted of TBBPA, TBBPA monomethyl ether, and an unknown polar compound. Our results indicated that bound-residue formation is the major pathway of TBBPA dissipation in oxic soil and provide first insights into the chemical structure of the reversibly ester-linked bound residues of TBBPA and its metabolites.


Assuntos
Ésteres/análise , Éter/análise , Bifenil Polibromatos/análise , Solo/química , Radioisótopos de Carbono , Substâncias Húmicas/análise , Hidrólise , Metaboloma , Poluentes do Solo/análise
14.
Environ Sci Technol ; 49(11): 6519-27, 2015 Jun 02.
Artigo em Inglês | MEDLINE | ID: mdl-25961764

RESUMO

A 6:2 chlorinated polyfluorinated ether sulfonate (6:2 Cl-PFAES) with the trade name F-53B, is an alternative to perfluorooctanesulfonate (PFOS) in electroplating industry that is uniquely used in China. It was developed as a mist suppressant initially in the 1970s, but the environmental behaviors and potential adverse effects of the 6:2 Cl-PFAES have only recently been investigated. In this work, the occurrence and distribution of perfluoroalkyl sulfonate (PFSA), fluorotelomer sulfonate (FTSA), and PFAES analogues were investigated in municipal sewage sludge samples collected around China. Perfluorobutane, perfluorohexane, perfluorooctane, and perfluorodecanesulfonates, 6:2 and 8:2 FTSAs, and the emerging 6:2 Cl-PFAES were detected. Moreover, 8:2 and 10:2 Cl-PFAESs were identified for the first time as new polyfluorinated contaminants using high resolution mass spectrometry. These fluorinated analytes were further quantified with the aid of commercial and laboratory-purified standards. PFOS was the predominant contaminant with a geometric mean (GM) value of 3.19 ng/g dry weight (d.w.), which was subsequently followed by 6:2 Cl-PFAES and 8:2 Cl-PFAES (GM: 2.15 and 0.50 ng/g d.w., respectively). Both 6:2 and 8:2 Cl-PFAES were positively detected as the major components in the F-53B commercial product, and discrete 6:2 Cl-PFAES/8:2 Cl-PFAES ratios in the product and sludge samples might suggest 8:2 Cl-PFAES had enhanced sorption behavior in the sludge due to the increase in hydrophobicity.


Assuntos
Ácidos Alcanossulfônicos/análise , Cidades , Éter/análise , Fluorocarbonos/análise , Esgotos/química , Poluentes Químicos da Água/análise , China , Meio Ambiente , Estatísticas não Paramétricas , Fatores de Tempo
15.
J Chromatogr A ; 1398: 83-93, 2015 Jun 12.
Artigo em Inglês | MEDLINE | ID: mdl-25913330

RESUMO

Countercurrent chromatography (CCC) is a technique, which uses two immiscible liquid phases for a separation process in a long and hollow tube. The technique allows the separation of high amounts of sample (50mg to several grams) with a low consumption of solvents. In this study, we fractionated 50mg technical octabromodiphenyl ether (DE-79) and analyzed the fractions by gas chromatography with mass spectrometry (GC/MS) and proton nuclear magnetic resonance ((1)H NMR) spectroscopy. CCC separations were performed with n-hexane/acetonitrile as solvent system in tail-to-head (i.e. the upper phase is mobile) mode. Twelve CCC fractions were studied for the PBDE composition. CCC elution of PBDE congeners was dependent both on the degree of bromination and substitution pattern. Higher brominated congeners eluted faster than lower brominated congeners and isomers with vicinal hydrogen atoms eluted last. In addition to several known PBDE congeners in DE-79, we were able to unequivocally identify BDE 195 in DE-79 and we could verify the presence of BDE 184. Finally, we also established the online hyphenation of CCC with (1)H NMR. The use of deuterated solvents could be avoided by using n-hexane/acetonitrile as two-phase system. By online CCC-(1)H NMR in stop-flow mode we were able to detect eight PBDE congeners in the mixture.


Assuntos
Técnicas de Química Analítica/métodos , Distribuição Contracorrente , Éter/química , Cromatografia Gasosa-Espectrometria de Massas , Espectroscopia de Ressonância Magnética , Fracionamento Químico , Éter/análise , Éteres/análise , Éteres Difenil Halogenados , Hexanos/química , Isomerismo , Solventes/química
16.
J Agric Food Chem ; 63(18): 4429-34, 2015 May 13.
Artigo em Inglês | MEDLINE | ID: mdl-25644932

RESUMO

A simple, fast, and cost-effective sample preparation method, previously developed and validated for the analysis of organic contaminants in fish using low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS), was evaluated for the analysis of polybrominated diphenyl ethers (PBDEs) and dichlorodiphenyltrichloroethane (DDT) pesticides using enzyme-linked immunosorbent assay (ELISA). The sample preparation technique was based on the quick, easy, cheap, rugged, effective, and safe (QuEChERS) approach with filter-vial dispersive solid phase extraction (d-SPE). Incurred PBDEs and DDTs were analyzed in three types of fish with 3-10% lipid content: Pacific croaker, salmon, and National Institute of Standards and Technology (NIST) Standard Reference Material 1947 (Lake Michigan fish tissue). LPGC-MS/MS and ELISA results were in agreement: 108-111 and 65-82% accuracy ELISA versus LPGC-MS/MS results for PBDEs and DDTs, respectively. Similar detection limits were achieved for ELISA and LPGC-MS/MS. Matrix effects (MEs) were significant (e.g., -60%) for PBDE measurement in ELISA, but not a factor in the case of DDT pesticides. This study demonstrated that the sample preparation method can be adopted for semiquantitative screening analysis of fish samples by commercial kits for PBDEs and DDTs.


Assuntos
Métodos Analíticos de Preparação de Amostras/métodos , DDT/isolamento & purificação , Éter/isolamento & purificação , Retardadores de Chama/isolamento & purificação , Contaminação de Alimentos/análise , Praguicidas/isolamento & purificação , Bifenil Polibromatos/isolamento & purificação , Alimentos Marinhos/análise , Animais , DDT/análise , Ensaio de Imunoadsorção Enzimática , Éter/análise , Peixes , Retardadores de Chama/análise , Cromatografia Gasosa-Espectrometria de Massas , Praguicidas/análise , Bifenil Polibromatos/análise
17.
Luminescence ; 30(3): 318-24, 2015 May.
Artigo em Inglês | MEDLINE | ID: mdl-24990144

RESUMO

A three-dimensional hierarchical CdO nanostructure with a novel bio-inspired morphology is reported. The field emission scanning electronic microscopy, transmission electron microscopy and X-ray diffractometer were employed to characterize the as-prepared samples. In gas-sensing measurements, acetone and diethyl ether were employed as target gases to investigate cataluminescence (CTL) sensing properties of the CdO nanostructure. The results show that the as-fabricated CdO nanostructure exhibited outstanding CTL properties such as stable intensity, high signal/noise values, short response and recovery time. The limit of detection of acetone and diethyl ether was ca. 6.5 ppm and 6.7 ppm, respectively, which was below the standard permitted concentrations. Additionally, a principal components analysis method was used to investigate the recognizable ability of the CTL sensor, and it was found that acetone and diethyl ether can be distinguished clearly. The performance of the bio-inspired CdO nanostructure-based sensor system suggested the promising application of the CdO nanostructure as a novel highly efficient CTL sensing material.


Assuntos
Acetona/análise , Compostos de Cádmio/química , Éter/análise , Medições Luminescentes/métodos , Nanoestruturas/química , Óxidos/química , Desenho de Equipamento , Limite de Detecção , Medições Luminescentes/instrumentação , Oxirredução , Análise de Componente Principal , Sensibilidade e Especificidade , Razão Sinal-Ruído , Temperatura , Difração de Raios X
18.
J Agric Food Chem ; 61(38): 9063-6, 2013 Sep 25.
Artigo em Inglês | MEDLINE | ID: mdl-24000828

RESUMO

MS with GC-RI evidence was found for the presence of linden ether in cooked carrot (Daucus carota). Evaluation of the GC effluent from cooked carrot volatiles using aroma extract dilution analysis (AEDA) found linden ether with the highest flavor dilution (FD) factor. Others with 10-fold lower FD factors were ß-ionone, eugenol, the previously unidentified ß-damascenone, (E)-2-nonenal, octanal (+ myrcene), and heptanal. All other previously identified volatiles showed lower FD factors. Odor thresholds, concentrations, and odor activity values of previously identified compounds are reviewed. This indicated that at least 20 compounds occur in cooked carrots above their odor thresholds (in water). Compounds showing the highest odor activity values included ß-damascenone, (E)-2-nonenal, (E,E)-2,4-decadienal, ß-ionone, octanal, (E)-2-decenal, eugenol, and p-vinylguaiacol.


Assuntos
Daucus carota/química , Éter/análise , Odorantes/análise , Extratos Vegetais/análise , Compostos Orgânicos Voláteis/análise , Culinária
19.
J Agric Food Chem ; 58(21): 11408-12, 2010 Nov 10.
Artigo em Inglês | MEDLINE | ID: mdl-20929232

RESUMO

In a large batch of ground hazelnuts, a metallic, solvent-like off-note was detected. In this investigation, the volatiles from the batch showing off-notes were compared to a batch without off-notes. On the basis of gas chromatography (GC) sniffing and instrumental analysis, a terpenoid compound, prenyl ethyl ether, was identified as a key contributor to the off-note. The compound was quantified, and its contribution to the metallic, solvent-like off-flavor was confirmed by spiking experiments and sensory evaluation. Analytical and sensory experiments found that the off-note was still present in hazelnut cakes. Fat oxidation did not contribute to the off-flavor. Analysis of market products demonstrated the correlation between the identified terpenoid and the off-flavor. It is assumed that fungi are involved in off-flavor formation.


Assuntos
Corylus/química , Éter/análise , Aromatizantes/análise , Neopreno/análise , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Paladar
20.
Anal Bioanal Chem ; 397(4): 1511-9, 2010 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-20401469

RESUMO

Open-path FT-IR spectra were measured while fireworks were emitting smoke and incandescent particles into the infrared beam. These conditions were designed to simulate the appearance of smoke and explosions in a battlefield. Diethyl ether was used to simulate the vapor-phase spectra of G agents such as sarin. The measured interferograms were corrected by a high-pass filter and were rejected when interfering features were of such high frequency that they could not be removed by application of this filter. The concentration of diethyl ether was calculated correctly by partial least squares regression in the absence of fireworks but significant errors were encountered when the spectra of the oxide particles were not included in the calibration set. Target factor analysis allowed the presence of the analyte to be detected even when the incandescent particles were present in the beam.


Assuntos
Atmosfera/análise , Substâncias para a Guerra Química/análise , Éter/análise , Espectroscopia de Infravermelho com Transformada de Fourier
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