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1.
Mikrochim Acta ; 188(10): 323, 2021 Sep 06.
Artigo em Inglês | MEDLINE | ID: mdl-34487246

RESUMO

The utilization of environmentally friendly nanoporous natural zeolite exchanged with Ni2+ ions (NiZ) and conductive carbon black (CB) in the fabrication of a novel and selective voltammetric sensor of vitamin B6 (VB6) is presented. The used clinoptilolite-rich zeolite material and CB were characterized in terms of morphology and textural properties. The superior properties of Ni-zeolite/carbon black modified glassy carbon electrode (NiZCB-GCE), arising from the synergistic effect of combining the unique features of zeolite and conductive carbon black, were confirmed by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements. In the determination of VB6 with the use of differential pulse voltammetry (DPV), the optimization of the pH value of supporting electrolyte and instrumental parameters, as well as the interference study were performed. Under optimized conditions, the oxidation peak current at the potential +0.72 V vs. Ag | AgCl | 3 M KCl reference electrode was linear to the VB6 concentration in the range 0.050 to 1.0 mg L-1 (0.30-5.9 µmol L-1) (R = 0.9993). The calculated limit of detection (LOD, S/N = 3), equal to 15 µg L-1 (0.09 µmol L-1), was much better compared to chemically modified electrodes with other carbon-based materials. The RSD for 0.5 mg L-1 was in the range 2.5-5.4% (n = 4). The developed NiZCB-GCE was successfully applied to the determination of VB6 in commercially available multivitamin dietary supplements, food, and water samples. The obtained recoveries ranged from 95 to 106%.


Assuntos
Técnicas Eletroquímicas/métodos , Nanocompostos/química , Fuligem/química , Vitamina B 6/análise , Zeolitas/química , Suplementos Nutricionais/análise , Bebidas Energéticas/análise , Limite de Detecção , Níquel/química , Porosidade , Águas Residuárias/análise
2.
Analyst ; 146(2): 612-619, 2021 Jan 21.
Artigo em Inglês | MEDLINE | ID: mdl-33185206

RESUMO

A glassy carbon electrode chemically modified with a carbon black coating is proposed here for the rapid and portable determination of cannabidiol (CBD) in a commercial Cannabis seed oil and in fibre-type Cannabis sativa L. leaves. The mechanism of CBD oxidation was studied in relation to simpler phenyl derivatives bearing the same electroactive group, namely resorcinol and 2-methylresorcinol. These molecules also allowed us to determine the best conditions for the electrochemical detection of CBD, as to the pH value and to the best solvent mixture to use. Carbon black was chosen among nanostructured carbon-based materials owing to its outstanding features as an electrode modifier for analyte detection. The performance of the modified electrode was determined by flow injection analyses of standard solutions of CBD, obtaining a linear correlation between the oxidation current and the analyte concentration; the sensor response is characterised by suitable repeatability and reproducibility. The analysis of commercial products by the standard addition method allowed us to ascertain the accuracy of the sensor for the detection of CBD in real samples.


Assuntos
Canabidiol/análise , Eletroquímica/instrumentação , Extratos Vegetais/química , Fuligem/química , Verduras/química , Canabidiol/química , Folhas de Planta/química , Água/química
3.
Mikrochim Acta ; 187(4): 216, 2020 03 11.
Artigo em Inglês | MEDLINE | ID: mdl-32162013

RESUMO

An integrated electrochemical immunoassay is described for the determination of circulating tumor cells (CTCs). For the first time, Ketjen black (KB), which is a superconductive carbon material, was incorporated with Au nanoparticles (AuNPs) and used to modify the surface of gold electrodes. A cocktail of anti-epithelial cell adhesion molecules (EpCAM) and anti-vimentin antibodies was chosen to capture the CTCs. Palladium-iridium-boron-phosphorus alloy-modified mesoporous nanospheres (PdIrBPMNS) served as a catalytic tag to amplify the current signal. Glycine-HCl (Gly-HCl) was used as an antibody eluent to release and collect the captured CTCs from the electrodes for further clinical research without compromising cell viability. The response of the method increased linearly from 10 to 1 × 106 cells mL-1 CTCs, while the detection limit was calculated to be as low as 2 cells mL-1. This method was successfully used to determine CTCs in spiked blood samples and demonstrated good recovery. Graphical abstractKetjen black/AuNPs was incorporated in the electrochemical platform to enhance the electron transfer ability of the electrode surface. PdIrBP mesoporous nanospheres were used to amplify DPV signal in this assay. The introduction of Gly-HCl realized nondestructive recovery of circulating tumor cells.


Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , Nanosferas/química , Células Neoplásicas Circulantes/patologia , Fuligem/química , Boro/química , Condutividade Elétrica , Humanos , Irídio/química , Paládio/química , Tamanho da Partícula , Fósforo/química , Porosidade , Propriedades de Superfície , Células Tumorais Cultivadas
4.
Mar Pollut Bull ; 146: 435-441, 2019 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-31426178

RESUMO

The sorption behavior of phosphorus onto sediment was investigated with the addition of BC derived from incomplete biomass combustion (PC). The sorption kinetic curves of phosphorus onto PC and sediment could be described by a two-compartment first order equation, and the sorption isotherms fit the Freundlich model well. With increasing amounts of PC added, the sorption capacity increased while the HI did not change much. The distribution of phosphorus forms showed that CaP (ACa-P plus DAP) constituted the highest fraction in the sediment samples. Throughout the sorption process, CaP and OP changed very little, but the Ex-P and FeP increased obviously, and the presence of PC made this increase more significantly. The high specific area and the presence of iron and aluminum, as well as the modification of the sediments surface properties, make the addition of PC be favorable for the sorption of phosphorus onto sediments.


Assuntos
Sedimentos Geológicos/química , Fósforo/química , Fuligem/química , Adsorção , Cinética , Propriedades de Superfície , Poluentes Químicos da Água/química
5.
Environ Pollut ; 249: 573-580, 2019 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-30933754

RESUMO

The adsorption of polycyclic aromatic hydrocarbons (PAHs) by components such as elemental carbon (EC), total organic carbon (TOC), and particles is different, and EC and PAHs are good materials for reconstructing historical human activity patterns and pollution conditions. In this study, the effects of EC (soot and char), TOC and particles of different grain size on PAHs in surface sediments were quantitatively analysed, and their historical concentrations in a sediment core from western Taihu Lake were reconstructed. The contents of soot, TOC, clay, EC and char explained 57.2%, 27.6%, 26.0%, 24.0% and 16.4%, respectively, of the PAH concentrations in surface sediments. The correlation between the soot and PAH levels was significantly higher than that between the char, TOC, and clay contents and PAH levels, and PAHs were mainly affected by the local economic development and human activity, as indicated by metrics of population, highway mileage, coal burning, and industrial output. With the development of the economy of the Taihu Lake Basin, the composition of PAHs in the sediments has changed: the proportion of low-molecular-weight PAHs decreased from 42.4% to 17.5%, and that of high-molecular-weight PAHs increased from 58.7% to 82.5%. The concentration of PAHs in pore water from Taihu Lake over the past 100 years was reconstructed and ranged from 43.1 to 961.2 µg L-1, with an average of 180.7 µg L-1. After China's reform and opening up, the concentrations of various PAHs in Taihu Lake changed from safe to chronic pollution levels. The ratios of lead (Pb) isotopes and the diagnostic ratios of PAHs showed that the main sources of PAHs in western Taihu Lake sediments were human activities such as coal and petroleum combustion.


Assuntos
Carbono/química , Monitoramento Ambiental/métodos , Poluição Ambiental/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Fuligem/química , Poluentes Químicos da Água/análise , China , Sedimentos Geológicos/química , Atividades Humanas , Lagos/química , Petróleo/análise , Solo/química
6.
Small ; 15(11): e1804575, 2019 03.
Artigo em Inglês | MEDLINE | ID: mdl-30761748

RESUMO

Herein, water-dispersible carbon nano-onion clusters (CNOCs) with an average hydrodynamic size of ≈90 nm are prepared by simply sonicating candle soot in a mixture of oxidizing acid. The obtained CNOCs have high photothermal conversion efficiency (57.5%), excellent aqueous dispersibility (stable in water for more than a year without precipitation), and benign biocompatibility. After polyethylenimine (PEI) and poly(ethylene glycol) (PEG) modification, the resultant CNOCs-PEI-PEG have a high photothermal conversion efficiency (56.5%), and can realize after-wash photothermal cancer cell ablation due to their ultrahigh cellular uptake (21.3 pg/cell), which is highly beneficial for the selective ablation of cancer cells via light-triggered intracellular heat generation. More interestingly, the cellular uptake of CNOCs-PEI-PEG is so high that the internalized nanoagents can be directly observed under a microscope without fluorescent labeling. Besides, in vivo experiments reveal that CNOCs-PEI-PEG can be used for photothermal/photoacoustic dual-modal imaging-guided photothermal therapy after intravenous administration. Furthermore, CNOCs-PEI-PEG can be efficiently cleared from the mouse body within a week, ensuring their excellent long-term biosafety. To the best of the authors' knowledge, the first example of using candle soot as raw material to prepare water-dispersible onion-like carbon nanomaterials for cancer theranostics is represented herein.


Assuntos
Carbono/química , Diagnóstico por Imagem , Hipertermia Induzida , Nanoestruturas/química , Neoplasias/terapia , Fototerapia , Fuligem/química , Água/química , Animais , Linhagem Celular Tumoral , Humanos , Camundongos , Nanoestruturas/ultraestrutura , Técnicas Fotoacústicas , Polietilenoglicóis/síntese química , Polietilenoglicóis/química , Polietilenoimina/síntese química , Polietilenoimina/química , Temperatura
7.
Skin Pharmacol Physiol ; 31(2): 87-94, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-29353285

RESUMO

BACKGROUND/AIMS: Airborne pollutants, such as nano-sized soot particles, are increasingly being released into the environment as a result of growing population densities and industrialization. They can absorb organic and metal compounds with potential biological activity, such as polycyclic aromatic hydrocarbons and airborne pollen allergens. Local and systemic toxicities may be induced in the skin if the particulates release their harmful components upon dermal contact. METHODS: In the present study, skin pretreatments with serum and/or shield as barrier formulations prior to exposure and washing with a cleanser subsequent to exposure were evaluated as a protection and decontamination strategy using laser scanning microscopy. RESULTS: The results indicate that while the application of serum and a cleanser was insufficient for decontamination, the pretreatment with shield prior to nanoparticle exposure followed by washing led to the removal of a considerable amount of the carbon black particles. The combined application of serum and shield before the administration of carbon black particles and subsequent washing led to their elimination from the skin samples. CONCLUSION: The application of barrier-enhancing formulations in combination with a cleanser may reduce the penetration of harmful airborne particulates by preventing their adhesion to the skin and facilitating their removal by subsequent washing with the cleanser.


Assuntos
Nanopartículas/química , Pele/química , Fuligem/química , Alérgenos/química , Animais , Descontaminação/métodos , Humanos , Lasers , Microscopia Confocal/métodos , Tamanho da Partícula , Pólen/química , Suínos
8.
PLoS One ; 12(2): e0158636, 2017.
Artigo em Inglês | MEDLINE | ID: mdl-28234998

RESUMO

Lamp illuminants evidence the exploitation of natural resources, animal and plant domestication, commerce, religious practices and nutrition of ancient populations. However, the physicochemical analysis of their major constituent-burned, degraded and aged mixture of triacylglycerols is imprecise and may lead to ambiguous interpretations. We applied proteomics to analyze fuel deposits from eight lamps dated by 6th to 8th centuries AD that were excavated at the Astana necropolis (Xinjiang, China) and determined their origin by identifying organism-specific proteins. Proteomics evidence corroborated and detailed the assignments of source organism relying upon comparative profiling of intact triacylglycerols by shotgun lipidomics. We found that ruminant (mostly, sheep) fat, cattle ghee and sesame oil were common combustibles in Astana and concluded that sesame as an oilseed appeared in China under Tang Dynasty concomitantly with the expansion of Buddhism.


Assuntos
Proteínas/química , Proteômica , Óleo de Gergelim/química , Fuligem/química , Animais , Bovinos , China , História Antiga , Humanos , Tinta , Paleontologia , Proteínas/isolamento & purificação , Ovinos
9.
Environ Sci Pollut Res Int ; 24(8): 7534-7543, 2017 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-28116624

RESUMO

A chemical characterization of diesel and hydrotreated vegetable oil (HVO) soot has been developed using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) before and after the reaction with different probe gases. Samples were generated under combustion conditions corresponding to an urban operation mode of a diesel engine and were reacted with probe gas-phase molecules in a Knudsen flow reactor. Specifically, NH2OH, O3 and NO2 were used as reactants (probes) and selected according to their reactivities towards specific functional groups on the sample surface. Samples of previously ground soot were diluted with KBr and were introduced in a DRIFTS accessory. A comparison between unreacted and reacted soot samples was made in order to establish chemical changes on the soot surface upon reaction. It was concluded that the interface of diesel and HVO soot before reaction mainly consists polycyclic aromatic hydrocarbons, nitro and carbonyl compounds, as well as ether functionalities. The main difference between both soot samples was observed in the band of the C=O groups that in diesel soot was observed at 1719 cm-1 but not in HVO soot. After reaction with probe gases, it was found that nitro compounds remain on the soot surface, that the degree of unsaturation decreases for reacted samples, and that new spectral bands such as hydroxyl groups are observed.


Assuntos
Óleos de Plantas , Fuligem , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Gases/química , Óleos de Plantas/análise , Óleos de Plantas/química , Hidrocarbonetos Policíclicos Aromáticos/química , Fuligem/análise , Fuligem/química
10.
Environ Sci Technol ; 50(6): 2946-55, 2016 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-26886850

RESUMO

Surface functional groups of two different types of combustion aerosols, a conventional diesel (EN 590) and a hydrotreated vegetable oil (HVO) soot, have been investigated using heterogeneous chemistry (i.e., gas-particle surface reactions). A commercial sample of amorphous carbon (Printex XE2-B) was analyzed as a reference substrate. A Knudsen flow reactor was used to carry out the experiments under molecular flow conditions. The selected gases for the titration experiments were: N(CH3)3 for the identification of acidic sites, NH2OH for the presence of carbonyl groups, CF3COOH and HCl for basic sites of different strength, and O3 and NO2 for reducing groups. Reactivity with N(CH3)3 indicates a lower density of acidic functionalities for Printex XE2-B in relation to diesel and HVO soot. Results for NH2OH experiments indicates that commercial amorphous carbon exhibits a lower abundance of available carbonyl groups at the interface compared to the results from diesel and HVO soot, the latter being the one with the largest abundance of carbonyl functions. Reactions with acids indicate the presence of weak basic oxides on the particle surface that preferentially interact with the strong acid CF3COOH. Finally, reactions with O3 and NO2 reveal that diesel and especially HVO have a significantly higher reactivity with both oxidizers compared to that of Printex XE2-B because they have more reducing sites by roughly a factor of 10 and 30, respectively. The kinetics of titration reactions have also been investigated.


Assuntos
Aerossóis/análise , Poluentes Atmosféricos/química , Fuligem/química , Emissões de Veículos/análise , Gases , Óleos de Plantas/química
11.
Environ Sci Technol ; 49(24): 14641-8, 2015 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-26551410

RESUMO

We investigated the effects of changing physiological conditions in the digestive tract expected with food ingestion on the apparent bioaccessibility (Bapp) of 11 polycyclic aromatic hydrocarbons (PAHs) in a fuel soot. A previously established in vitro digestive model was applied that included silicone sheet as a third-phase absorptive sink simulating passive transfer of PAHs to intestinal epithelium in the small intestine stage. The Bapp is defined as the fraction found in the digestive fluid plus sheet after digestion. We determined that Bapp was independent of gastric pH and addition of nonlipid milk representing dietary proteins and carbohydrates, whereas it increased with bile acids concentration (2.0-10 g/L), small intestinal pH (5.00-7.35), and addition of soybean oil representing dietary lipid (100% and 200% of the mean daily ingestion by 2-5 year olds in the U.S.). Bapp of PAHs increases with small intestinal pH due to the combined effects of mass transfer promotion from nonlabile to labile sorbed states in the soot, weaker sorption of the labile state, and increasingly favorable partitioning from the digestive fluid to the silicone sink. Under fed conditions, Bapp increases with inclusion of lipids due to the combined effects of mass transfer promotion from nonlabile to labile states, and increasingly favorable partitioning into bile acid micelles. Our results indicate significant variability in soot PAH bioaccessibility within the range of physiological conditions experienced by humans, and suggest that bioaccessibility will increase with coconsumption of food, especially food with high fat content.


Assuntos
Ingestão de Alimentos , Intestino Delgado/fisiologia , Hidrocarbonetos Policíclicos Aromáticos/farmacocinética , Fuligem/química , Ácidos e Sais Biliares , Disponibilidade Biológica , Digestão/fisiologia , Trato Gastrointestinal/metabolismo , Humanos , Concentração de Íons de Hidrogênio , Intestino Delgado/metabolismo , Modelos Biológicos , Hidrocarbonetos Policíclicos Aromáticos/análise , Silicones , Óleo de Soja/farmacologia
12.
J Contam Hydrol ; 177-178: 194-205, 2015.
Artigo em Inglês | MEDLINE | ID: mdl-25977994

RESUMO

The aim of this study was to investigate the transport behavior of carboxyl-functionalized carbon black nanoparticles (CBNPs) in porous media including quartz sand, iron oxide-coated sand (IOCS), and aluminum oxide-coated sand (AOCS). Two sets of column experiments were performed under saturated flow conditions for potassium chloride (KCl), a conservative tracer, and CBNPs. Breakthrough curves were analyzed to obtain mass recovery and one-dimensional transport model parameters. The first set of experiments was conducted to examine the effects of metal (Fe, Al) oxides and flow rate (0.25 and 0.5 mL min(-1)) on the transport of CBNPs suspended in deionized water. The results showed that the mass recovery of CBNPs in quartz sand (flow rate=0.5 mL min(-1)) was 83.1%, whereas no breakthrough of CBNPs (mass recovery=0%) was observed in IOCS and AOCS at the same flow rate, indicating that metal (Fe, Al) oxides can play a significant role in the attachment of CBNPs to porous media. In addition, the mass recovery of CBNPs in quartz sand decreased to 76.1% as the flow rate decreased to 0.25 mL min(-1). Interaction energy profiles for CBNP-porous media were calculated using DLVO theory for sphere-plate geometry, demonstrating that the interaction energy for CBNP-quartz sand was repulsive, whereas the interaction energies for CBNP-IOCS and CBNP-AOCS were attractive with no energy barriers. The second set of experiments was conducted in quartz sand to observe the effect of ionic strength (NaCl=0.1 and 1.0mM; CaCl2=0.01 and 0.1mM) and pH (pH=4.5 and 5.4) on the transport of CBNPs suspended in electrolyte. The results showed that the mass recoveries of CBNPs in NaCl=0.1 and 1.0mM were 65.3 and 6.4%, respectively. The mass recoveries of CBNPs in CaCl2=0.01 and 0.1mM were 81.6 and 6.3%, respectively. These results demonstrated that CBNP attachment to quartz sand can be enhanced by increasing the electrolyte concentration. Interaction energy profiles demonstrated that the interaction energy profile for CBNP-quartz sand was compressed and that the energy barrier decreased as the electrolyte concentration increased. Furthermore, the mass recovery of CBNPs in the presence of divalent ions (CaCl2=0.1 mM) was far lower than that in the presence of monovalent ions (NaCl=0.1 mM), demonstrating a much stronger effect of Ca(2+) than Na(+) on CBNP transport. Mass recovery of CBNPs at pH 4.5 was 55.6%, which was lower than that (83.1%) at pH 5.4, indicating that CBNP attachment to quartz sand can be enhanced by decreasing the pH. The sticking efficiencies (α) calculated from the mass recovery by colloid filtration theory were in the range from 2.1×10(-2) to 4.5×10(-1), which were far greater than the values (2.56×10(-6)-3.33×10(-2)) of theoretical sticking efficiencies (αtheory) calculated from the DLVO energy by the Maxwell model.


Assuntos
Modelos Teóricos , Nanopartículas , Fuligem , Óxido de Alumínio/química , Coloides , Compostos Férricos/química , Concentração de Íons de Hidrogênio , Hidrologia/métodos , Nanopartículas/química , Concentração Osmolar , Porosidade , Quartzo , Dióxido de Silício , Poluentes do Solo/química , Fuligem/química , Água , Poluentes Químicos da Água/química
13.
J Environ Sci (China) ; 28: 171-7, 2015 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-25662252

RESUMO

Binary oxide systems (CuCr2O4, CuCo2O4), deposited onto cordierite monoliths of honeycomb structure with a second support (finely dispersed Al2O3), were prepared as filters for catalytic combustion of diesel soot using internal combustion engine's gas exhausts (O2, NOx, H2O, CO2) and O3 as oxidizing agents. It is shown that the second support increases soot capacity of aforementioned filters, and causes dispersion of the particles of spinel phases as active components enhancing thereby catalyst activity and selectivity of soot combustion to CO2. Oxidants used can be arranged with reference to decreasing their activity in a following series: O3≫NO2>H2O>NO>O2>CO2. Ozone proved to be the most efficient oxidizing agent: the diesel soot combustion by O3 occurs intensively (in the presence of copper chromite based catalyst) even at closing to ambient temperatures. Results obtained give a basis for the conclusion that using a catalytic coating on soot filters in the form of aforementioned binary oxide systems and ozone as the initiator of the oxidation processes is a promising approach in solving the problem of comprehensive purification of automotive exhaust gases at relatively low temperatures, known as the "cold start" problem.


Assuntos
Poluentes Atmosféricos/química , Poluição do Ar/prevenção & controle , Recuperação e Remediação Ambiental/métodos , Fuligem/química , Óxido de Alumínio/química , Compostos de Cromo/química , Cobre/química , Óxido de Magnésio/química , Minerais/química , Oxirredução , Emissões de Veículos/análise
14.
J Phys Chem A ; 117(48): 12897-911, 2013 Dec 05.
Artigo em Inglês | MEDLINE | ID: mdl-24188183

RESUMO

The heterogeneous reactions between trace gases and aerosol surfaces have been widely studied over the past decades, revealing the crucial role of these reactions in atmospheric chemistry. However, existing knowledge on the reactivity of mixed aerosols is limited, even though they have been observed in field measurements. In the current study, the heterogeneous interaction of NO2 with solid surfaces of Al2O3 covered with kerosene soot was investigated under dark conditions and in the presence of UV light. Experiments were performed at 293 K using a low-pressure flow-tube reactor coupled with a quadrupole mass spectrometer. The steady-state uptake coefficient, γ(ss), and the distribution of the gas-phase products were determined as functions of the Al2O3 mass; soot mass; NO2 concentration, varied in the range of (0.2-10) × 10(12) molecules cm(-3); photon flux; and relative humidity, ranging from 0.0032% to 32%. On Al2O3/soot surfaces, the reaction rate was substantially increased, and the formation of HONO was favored compared with that on individual pure soot and pure Al2O3 surfaces. Uptake of NO2 was enhanced in the presence of H2O under both dark and UV irradiation conditions, and the following empirical expressions were obtained: γ(ss,BET,dark) = (7.3 ± 0.9) × 10(-7) + (3.2 ± 0.5) × 10(-8) × RH and γ(ss,BET,UV) = (1.4 ± 0.2) × 10(-6) + (4.0 ± 0.9) × 10(-8) × RH. Specific experiments, with solid sample preheating and doping with polycyclic aromatic hydrocarbons (PAHs), showed that UV-absorbing organic compounds significantly affect the chemical reactivity of the mixed mineral/soot surfaces. A mechanistic scheme is proposed, in which Al2O3 can either collect electrons, initiating a sequence of redox reactions, or prevent the charge-recombination process, extending the lifetime of the excited state and enhancing the reactivity of the organics. Finally, the atmospheric implications of the observed results are briefly discussed.


Assuntos
Óxido de Alumínio/química , Atmosfera/química , Dióxido de Nitrogênio/química , Fuligem/química , Raios Ultravioleta , Propriedades de Superfície
15.
Anal Bioanal Chem ; 405(1): 389-400, 2013 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-23070044

RESUMO

Different extraction methods, followed by gas chromatography coupled to triple quadrupole mass spectrometry, were evaluated for simultaneous extraction of seven polychlorinated biphenyls (PCBs) and six polybrominated diphenyl ethers (PBDEs) from common weeds. Pressurized liquid extraction (PLE) with in-cell clean-up, ultrasound-assisted extraction (UAE) with in-column clean-up, and UAE with dispersive solid-phase extraction (dSPE) clean-up were evaluated and compared. In-cell clean-up with 4 g Florisil and 0.5 g graphitized carbon black (GCB) and two extraction cycles of 10 min with n-hexane-ethyl acetate 80:20 (v/v) at 60 °C were used for the PLE procedure. UAE with in-column clean-up was conducted under conditions similar to those reported for the PLE method whereas in UAE with dSPE clean-up purification of the extract was performed after extraction using primary and secondary amine sorbent (PSA) and GCB. Recovery from 82 to 104% was obtained for all the compounds by PLE whereas, in general, lower extraction efficiency was obtained by UAE with in-column clean-up (especially for BDE-17 and BDE-183, for which recovery was 70 and 41%, respectively) and by UAE with dSPE clean-up, for which the main drawback is that BDE-183 cannot be extracted. Finally, PLE was used for analysis of PCBs and PBDEs in different plants (Lolium rigidum, Lactuca serriola, Malva sylvestris, and Verbascum thapsus) collected from residential and/or rural areas of Madrid (Spain). Several of the analyzed compounds were detected at low levels in these plants, but only PCB-153 could be quantified.


Assuntos
Técnicas de Química Analítica/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Halogênios/análise , Extratos Vegetais/metabolismo , Poluentes do Solo/análise , Compostos de Bifenilo/química , Calibragem , Desenho de Equipamento , Peso Molecular , Extratos Vegetais/química , Plantas/metabolismo , Bifenilos Policlorados/análise , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos , Solventes/química , Fuligem/química , Espanha , Espectrometria de Massas em Tandem/métodos , Temperatura , Fatores de Tempo
16.
J Agric Food Chem ; 60(16): 4026-33, 2012 Apr 25.
Artigo em Inglês | MEDLINE | ID: mdl-22480352

RESUMO

A method for analysis of 37 pesticide residues in tea samples was developed and validated and was based on reversed-dispersive solid-phase extraction (r-DSPE) cleanup in acetonitrile solution, followed by liquid chromatography-electrospray tandem mass spectrometry determination. Green tea, oolong tea, and puer tea were selected as matrixes and represent the majority of tea types. Acetonitrile was used as the extraction solvent, with sodium chloride and magnesium sulfate enhancing partitioning of analytes into the organic phase. The extract was then cleaned up by r-DSPE using a mixture of multiwalled carbon nanotubes, primary secondary amine, and graphitized carbon black as sorbents to absorb interferences. Further optimization of sample preparation and determination allowed recoveries of between 70% and 111% for all 37 pesticides with relative standard deviations lower than 14% at two concentration levels of 10 and 100 µg kg(-1). Limits of quantification ranged from 5 to 20 µg kg(-1) for all pesticides. The developed method was successfully applied to the determination of pesticide residues in market tea samples.


Assuntos
Camellia sinensis/química , Contaminação de Alimentos/análise , Resíduos de Praguicidas/análise , Resíduos de Praguicidas/isolamento & purificação , Extração em Fase Sólida/métodos , Chá/química , Acetonitrilas/química , Adsorção , Aminas/química , Cromatografia Gasosa-Espectrometria de Massas , Nanotubos de Carbono/química , Extração em Fase Sólida/instrumentação , Fuligem/química
17.
Talanta ; 88: 445-9, 2012 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-22265524

RESUMO

A simple procedure for the modification of carbon nanoparticles (CNPs) from castor oil soot using acid treatment was described herein. Characterization studies revealed the presence of edge plane sites and surface carbon-oxygen functionalities at the surface of the CNP material. Voltammetric studies revealed the increased electrochemical activity of the CNP-modified electrode toward various biologically important molecules, including dopamine, uric acid, dihydronicotinamide adenine dinucleotide, tyrosine, and serotonin, relative to those obtained using the unmodified electrode. The improved electro-oxidation potentials for these compounds-and, thereby, the enhanced sensitivity of related sensors-was due directly to the presence of surface C(δ+)O(δ-) functional groups and the greater number of edge plane sites developed after acid treatment of the soot sample.


Assuntos
Carbono/química , Óleo de Rícino/química , Nanopartículas/química , Fuligem/química , Ácido Ascórbico/análise , Dopamina/análise , Eletroquímica , Eletrodos , Microscopia Eletrônica de Transmissão , NAD/análise , Nanopartículas/ultraestrutura , Oxirredução , Oxigênio/química , Espectroscopia Fotoeletrônica , Serotonina/análise , Espectroscopia de Infravermelho com Transformada de Fourier , Tirosina/análise , Ácido Úrico/análise
18.
J Hazard Mater ; 187(1-3): 283-90, 2011 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-21276659

RESUMO

MnO(x)-CeO(2)-Al(2)O(3) mixed oxides were prepared by impregnating manganese acetate and cerium nitrate on alumina powders using the sol-gel method. The thermal stabilities of MnO(x)-CeO(2) and Al(2)O(3)-modified mixed oxides were evaluated by treating at 800 °C in dry air flow for 20h. The introduction of Al(2)O(3) markedly increases the textural stability of the catalyst with a relatively high dispersion of MnO(x) and CeO(2), remaining a strong synergistic effect between these two oxides. The NO oxidation activity of the ternary oxides experiences a smaller loss after high-temperature calcination, and a low soot oxidation temperature is attained in the presence of NO.


Assuntos
Óxido de Alumínio/química , Cério/química , Compostos de Manganês/química , Óxidos/química , Fuligem/química , Catálise , Oxirredução , Temperatura , Difração de Raios X
19.
J Food Sci ; 74(8): S345-50, 2009 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-19799679

RESUMO

UNLABELLED: In this study, photooxidation of sour cream packaged in cups with different light barrier properties was investigated. The sour cream was light exposed for 36 h with a standard fluorescent light tube, simulating storage conditions in many Norwegian grocery stores. Three different cups were evaluated: a white cup, a cup with medium light barrier (LB), and a cup with high LB. The quality of the sour cream was evaluated by sensory analysis and front face fluorescence spectroscopy. The sour cream stored in white cups became very rancid during the light exposure, with a rancid flavor score of 7.8 on a scale from 1 to 9, where 9 is the highest intensity. Cups with high LB gave best protection against the light. The sensory assessors could not distinguish between sour cream stored in cups with high LB and sour cream stored in the dark. The rancid flavor intensity for the cups with medium LB was significantly different (P < 0.05) from both the white cup and the cup with high LB. The sensory flavor intensities indicated that with 36 h of light exposure, only a cup with high LB will protect the sour cream sufficiently. The fluorescence measurements corresponded well with the sensory analysis as the photosensitizers were somewhat degraded for sour cream stored in cups with medium LB and most degraded in the white cups. For the cups with high LB, the fluorescence peaks that originated from the photosensitizers were all intact. PRACTICAL APPLICATION: Dairy products such as sour cream will develop off-odor and taste faults ("sunlight taste") in a few hours if exposed to sufficient fluorescent lightning in the grocery stores. A light barrier can be incorporated in the packaging material to protect the dairy products from the light. Our experiment showed that the incorporation of a black pigment into 1 of the 3 plastic layers in the cup for packaging of sour cream protected the sour cream from degradation when exposed to light.


Assuntos
Produtos Fermentados do Leite/química , Produtos Fermentados do Leite/normas , Embalagem de Alimentos/instrumentação , Luz , Fotólise , Óxido de Alumínio/química , Animais , Produtos Fermentados do Leite/efeitos da radiação , Análise de Alimentos , Manipulação de Alimentos/métodos , Odorantes/análise , Oxirredução/efeitos da radiação , Poliestirenos/química , Controle de Qualidade , Fuligem/química , Espectrometria de Fluorescência , Espectrofotometria , Paladar , Titânio/química
20.
J Hazard Mater ; 161(1): 366-72, 2009 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-18462875

RESUMO

A series of potassium-promoted hydrotalcite-based CoMgAlO mixed oxide catalysts used for simultaneous soot combustion and nitrogen oxides storage were prepared by impregnation method. The techniques of TG/DTA, XRD, H2-TPR and in situ DRIFTS were employed for catalyst characterization. Over the catalyst containing 7.5% or 10% K, the soot ignition temperature (Ti=260 degrees C) and total removal temperature (Tf=390 degrees C) are decreased by 180 degrees C and 273 degrees C, respectively, as compared with the uncatalyzed reaction. The results of kinetic calculation show that the presence of K-promoted catalysts decreases the activation energy of soot combustion from 207kJ/mol to about 160kJ/mol. When 400ppm NO is introduced, lower characteristic temperatures or higher reaction rate for soot oxidation is achieved. Simultaneously, relatively larger nitrogen oxides storage capacity is obtained. It is revealed by H2-TPR that the addition of K increases the amount of active Co sites and the mobility of bulk lattice oxygen due to the low melting point of K-containing compounds, the low valence of K+ and the strong interaction between K and Mg(Al). For nitrogen oxides storage, different routes via chelating bidentate nitrates, monodentate nitrates and ionic nitrates are confirmed by in situ DRIFTS over the CoMgAlO catalysts with potassium loadings of 0, 1.5 and 7.5%, respectively.


Assuntos
Hidróxido de Alumínio/química , Óxido de Alumínio/química , Hidróxido de Magnésio/química , Óxidos de Nitrogênio/química , Potássio/química , Fuligem/química , Catálise , Estrutura Molecular , Análise Espectral , Temperatura , Difração de Raios X
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