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1.
Environ Res ; 252(Pt 4): 119121, 2024 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-38734291

RESUMO

Extensive utilization of pesticides and herbicides to boost agricultural production increased the environmental health risks, which can be mitigate with the aid of highly sensitive detection systems. In this study, an electrochemical sensor for monitoring the carcinogenic pesticides in the environmental samples has been developed based on sulfur-doped graphitic-carbon nitride-gold nanoparticles (SCN-AuNPs) nanohybrid. Thermal polycondensation of melamine with thiourea followed by solvent exfoliation via ultrasonication leads to SCN formation and electroless deposition of AuNPs on SCN leads to SCN-AuNPs nanohybrid synthesis. The chemical composition, S-doping, and the morphology of the nanohybrid were confirmed by various microscopic and spectroscopic tools. The as-synthesized nanohybrid was fabricated with glassy carbon (GC) electrode for determining the carcinogenic hydrazine (HZ) and atrazine (ATZ) in field water samples. The present sensor exhibited superior electrocatalytic activity than GC/SCN and GC/AuNPs electrodes due to the synergism between SCN and AuNPs and the amperometric studies showed the good linear range of detection of 20 nM-0.5 mM and 500 nM-0.5 mM with the limit of detection of 0.22 and 69 nM (S/N = 3) and excellent sensitivity of 1173.5 and 13.96 µA mM-1 cm-2 towards HZ and ATZ, respectively. Ultimately, the present sensor is exploited in environmental samples for monitoring HZ and ATZ and the obtained results are validated with high-performance liquid chromatography (HPLC) technique. The excellent recovery percentage and close agreement with the results of HPLC analysis proved the practicability of the present sensor. In addition, the as-prepared materials were utilized for the photocatalytic degradation of ATZ and the SCN-AuNPs nanohybrid exhibited higher photocatalytic activity with the removal efficiency of 93.6% at 90 min. Finally, the degradation mechanism was investigated and discussed.


Assuntos
Carcinógenos , Ouro , Grafite , Nanopartículas Metálicas , Poluentes Químicos da Água , Ouro/química , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química , Nanopartículas Metálicas/química , Grafite/química , Carcinógenos/análise , Atrazina/análise , Atrazina/química , Enxofre/química , Enxofre/análise , Técnicas Eletroquímicas/métodos , Hidrazinas/análise , Hidrazinas/química , Compostos de Nitrogênio/química , Compostos de Nitrogênio/análise , Nitrilas/química , Nitrilas/análise , Monitoramento Ambiental/métodos
2.
J Occup Environ Hyg ; 16(1): 78-88, 2019 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-30335595

RESUMO

Personnel in swimming pool facilities typically experience ocular, nasal, and respiratory symptoms due to water chlorination and consequent exposure to disinfection by-products in the air. The aim of the study was to investigate exposure to trichloramine and trihalomethanes (chloroform, bromodichloromethane, dibromochloromethane, and bromoform) from the perspective of adverse health effects on the personnel at Swedish habilitation and rehabilitation swimming pools. The study included 10 habilitation and rehabilitation swimming pool facilities in nine Swedish cities. The study population comprised 24 exposed swimming pool workers and 50 unexposed office workers. Personal and stationary measurements of trichloramine and trihalomethanes in air were performed at all the facilities. Questionnaires were distributed to exposed workers and referents. Spirometry, fraction of exhaled nitric oxide (FENO), and peak expiratory flow (PEF) were measured. Personal and stationary measurements yielded trichloramine levels of 1-76 µg/m3 (average: 19 µg/m3) and 1-140 µg/m3 (average: 23 µg/m3), respectively. A slightly higher, but not significant, prevalence of reported eye- and throat-related symptoms occurred among the exposed workers than among the referents. A significantly increased risk of at least one ocular symptom was attributed to trichloramine exposure above the median (20 µg/m3). Lung function (FVC and FEV1) was in the normal range according to the Swedish reference materials, and no significant change in lung function before and after shift could be established between the groups. Average FENO values were in the normal range in both groups, but the difference in the values between the exposed workers and referents showed a significant increase after shift. Hourly registered PEF values during the day of the investigation did not show any unusual individual variability. In conclusion, the increased risk of developing at least one ocular symptom at personal trichloramine concentrations over 20 µg/m3 combined with an increase in the difference in FENO during the work shift of the exposed workers should not be neglected as an increased risk of respiratory inflammation in the habilitation and rehabilitation swimming pool environment.


Assuntos
Poluição do Ar em Ambientes Fechados/análise , Cloretos/análise , Compostos de Nitrogênio/análise , Exposição Ocupacional/análise , Piscinas , Trialometanos/análise , Adulto , Poluição do Ar em Ambientes Fechados/efeitos adversos , Cloretos/efeitos adversos , Estudos Transversais , Desinfetantes/efeitos adversos , Desinfetantes/análise , Olho/efeitos dos fármacos , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Compostos de Nitrogênio/efeitos adversos , Centros de Reabilitação , Testes de Função Respiratória , Suécia , Trialometanos/efeitos adversos
3.
Pesqui. vet. bras ; 37(8): 883-890, Aug. 2017. tab
Artigo em Português | LILACS, VETINDEX | ID: biblio-895494

RESUMO

Avaliou-se o efeito da inclusão da silagem da raiz de mandioca sobre os parâmetros ruminais e o balanço de compostos nitrogenados em bovinos de origem leiteira. Utilizou-se cinco animais, canulados no rúmen, não lactantes e com peso corporal médio de 389 kg. Os animais foram distribuídos em um quadrado latino cinco x cinco, sendo cinco dietas com níveis de inclusão (0,00; 3,62; 7,23; 10,84; e 14,54% da matéria seca da dieta) da silagem da raiz de mandioca e cinco períodos. Cada período constituiu-se em 10 dias de adaptação e cinco dias para a coleta dos dados. As excreções de nitrogênio na urina e nas fezes não foram influenciadas (P>0,05) pela inclusão da silagem da raiz de mandioca nas dietas. O consumo de nitrogênio total (CNT) e o balanço de nitrogênio (BN) apresentaram comportamento quadrático e linear crescente, respectivamente. Obteve-se o menor CNT (142,14 g/dia) no nível de inclusão de 5,82% de silagem da raiz de mandioca. As concentrações de ureia (U) e de nitrogênio ureico (NU) na urina e no plasma não modificaram (P>0,05). Observou-se comportamento quadrático (P<0,05) nas excreções de U e NU na urina, com ponto de mínimo de 131,13 e 61,20 g/dia, respectivamente, no nível de 7,27% de inclusão da silagem da raiz de mandioca. Não houve interação (P>0,05) entre os níveis da silagem da raiz de mandioca e o tempo de coleta do conteúdo ruminal para os ácidos graxos de cadeia curta, o pH e o nitrogênio amoniacal (N-NH3). Apenas o teor de N-NH3 apresentou comportamento quadrático, em função dos níveis de inclusão, obtendo-se o ponto mínimo (12,62 mg/100 mL de conteúdo ruminal) no nível de 5,98%. O nível de 7,23% de silagem da raiz de mandioca na dieta foi mais eficiente na utilização dos compostos nitrogenados. As dietas contribuem de forma semelhante para a produção dos ácidos graxos de cadeia curta, sem interferir no pH ruminal.(AU)


The effect of inclusion of cassava root silage on ruminal parameters and nitrogenous compounds in dairy cattle was evaluated. Five cattle cannulated in the rumen and with average body weight of 389 kg were distributed into a Latin square 5x5, with five levels of inclusion (0.00, 3.62, 7.23, 10.84 and 14.54% of the diet dry matter) of cassava root silage and five periods (10 days for adaptation and five days for data collection). The nitrogen excretion in urine and feces were not affected (P>0.05) by inclusion of cassava root silage in the diet. The total nitrogen intake (CNT) and nitrogen balance (NB) showed an increasing quadratic and linear behavior, respectively. The lowest CNT (142.14g/day) was obtained with the inclusion of 5.82% silage cassava root. The concentration of urea (U) and urea nitrogen (UN) in plasma and urine did not change (P>0.05). There was a quadratic behavior (P<0.05) in excreta of U and NU in the urine, with minimum point of 131.13 and 61.20g/day respectively, at the level of 7.27% inclusion of the cassava root silage. No interaction (P>0.05) was between the levels of cassava root silage and the collection time of rumen contents for the short-chain fatty acids, pH and ammonia nitrogen (NH3-N). Only the N-NH3 protein showed quadratic behavior, according to the inclusion levels, with the minimum point (12.62mg/100ml of rumen contents) at the level of 5.98%. The level of 7.23% of cassava root silage in the diet was more efficient with the use of nitrogen compounds. The diets contribute similarly to the production of short chain fatty acids, without disturbing the rumen pH.(AU)


Assuntos
Animais , Bovinos , Rúmen/química , Silagem/análise , Amido , Manihot , Compostos de Nitrogênio/análise , Saccharum
4.
Eur J Mass Spectrom (Chichester) ; 23(2): 83-88, 2017 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-28657415

RESUMO

We report the investigation of the hydrothermal liquefaction products of the Spirulina platensis microalgae by using the Fourier transform ion cyclotron resonance mass spectrometry. The hydrothermal liquefaction produced two fractions: one with boiling temperature below 300℃ and the dense residue that remained in the reactor. It was observed that N2 and N classes of compounds that dominate in the positive ESI Fourier transform ion cyclotron resonance spectra for both fractions, and that the light fraction is considerably more saturated then the heavy one. The performed hydrogen/deuterium exchange reaction indicated the presence of the onium compounds in the bio-oil.


Assuntos
Biocombustíveis/análise , Ciclotrons , Compostos de Nitrogênio/análise , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Spirulina/química , Calefação/métodos , Compostos de Nitrogênio/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Temperatura
5.
Anim Sci J ; 88(2): 379-385, 2017 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-27169902

RESUMO

We evaluated the enhancement of cured meat taste during maturation by sensory analysis. We focused on the heat-stable sarcoplasmic fraction (HSSF) to identify the factors related to cured meat taste. Because the dry matter of HSSF contained more than 30% nitrogen, nitrogen compounds such as free amino acids, small peptides and adenosine triphosphate-related compounds seemed to be the important components of HSSF. The samples cured with HSSF for 2 h exhibited the same taste profile as ones cured without HSSF for 168 h. Therefore, the changes in the amount and fractions of nitrogen compounds were examined in HSSF during incubation from 0 to 168 h. The concentration of hypoxanthine (Hx) gradually increased, while inosine-5'-monophosphate decreased during the incubation. The samples cured with pickles containing various concentrations of Hx were subjected to sensory analysis. The addition of Hx, in a dose-dependent fashion, enhanced cured meat taste by maturation for 2 h. It was concluded that Hx is essential for the enhancement of cured meat taste.


Assuntos
Manipulação de Alimentos/métodos , Qualidade dos Alimentos , Hipoxantina/análise , Produtos da Carne , Carne , Paladar , Trifosfato de Adenosina/análise , Aminoácidos/análise , Humanos , Carne/análise , Produtos da Carne/análise , Nitrogênio/análise , Compostos de Nitrogênio/análise , Peptídeos/análise , Fatores de Tempo
6.
Nat Mater ; 16(2): 264-272, 2017 02.
Artigo em Inglês | MEDLINE | ID: mdl-27798623

RESUMO

Plant nanobionics aims to embed non-native functions to plants by interfacing them with specifically designed nanoparticles. Here, we demonstrate that living spinach plants (Spinacia oleracea) can be engineered to serve as self-powered pre-concentrators and autosamplers of analytes in ambient groundwater and as infrared communication platforms that can send information to a smartphone. The plants employ a pair of near-infrared fluorescent nanosensors-single-walled carbon nanotubes (SWCNTs) conjugated to the peptide Bombolitin II to recognize nitroaromatics via infrared fluorescent emission, and polyvinyl-alcohol functionalized SWCNTs that act as an invariant reference signal-embedded within the plant leaf mesophyll. As contaminant nitroaromatics are transported up the roots and stem into leaf tissues, they accumulate in the mesophyll, resulting in relative changes in emission intensity. The real-time monitoring of embedded SWCNT sensors also allows residence times in the roots, stems and leaves to be estimated, calculated to be 8.3 min (combined residence times of root and stem) and 1.9 min mm-1 leaf, respectively. These results demonstrate the ability of living, wild-type plants to function as chemical monitors of groundwater and communication devices to external electronics at standoff distances.


Assuntos
Engenharia Genética/métodos , Hidrocarbonetos Aromáticos/metabolismo , Compostos de Nitrogênio/metabolismo , Peptídeos/metabolismo , Plantas Geneticamente Modificadas/fisiologia , Spinacia oleracea/fisiologia , Biônica/métodos , Substâncias Explosivas/análise , Hidrocarbonetos Aromáticos/análise , Raios Infravermelhos , Nanotubos de Carbono/química , Compostos de Nitrogênio/análise , Peptídeos/genética
7.
J Biosci Bioeng ; 123(3): 327-332, 2017 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-27784621

RESUMO

High-salt content seaweed sauces were prepared for the first time using nori (Pyropia yezoensis) by fermentation and characterized. Components and taste of the two nori sauces (NSs) prepared separately were compared with those of soy and fish sauces. The NSs were rich in total nitrogen compounds (1.5 g N/100 ml on average) and potassium (880 mg/100 g), and had a unique free amino acid composition (e.g., taurine 617 mg/100 g), explaining their unique taste as evaluated by a taste sensing system. As for their food function, inhibitory activity of angiotensin-converting enzyme was observed. As for their food safety, arsenic was detected at a 0.8 mg/100 g level in total, but inorganic arsenic was not detected (<0.05 mg/100 g) and not regarded as a problem. Allergy-causing substances contained in wheat, soy beans, and crustaceans were not detected (<0.1 mg/100 g) with NSs. These results suggest that the nori sauce has a high potential as a novel nutritional source for humans.


Assuntos
Condimentos/análise , Fermentação , Análise de Alimentos , Porphyra/química , Alga Marinha/química , Alérgenos/análise , Aminoácidos/análise , Arsênio/análise , Reatores Biológicos , Humanos , Compostos de Nitrogênio/análise , Potássio/análise , Cloreto de Sódio/análise , Alimentos de Soja/análise
8.
J Chromatogr A ; 1461: 131-43, 2016 Aug 26.
Artigo em Inglês | MEDLINE | ID: mdl-27488721

RESUMO

Diesel and naphtha samples were analyzed using ionic liquid (IL) columns to evaluate the best column set for the investigation of organic sulfur compounds (OSC) and nitrogen(N)-containing compounds analyses with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry detector (GC×GC/TOFMS). Employing a series of stationary phase sets, namely DB-5MS/DB-17, DB-17/DB-5MS, DB-5MS/IL-59, and IL-59/DB-5MS, the following parameters were systematically evaluated: number of tentatively identified OSC, 2D chromatographic space occupation, number of polyaromatic hydrocarbons (PAH) and OSC co-elutions, and percentage of asymmetric peaks. DB-5MS/IL-59 was chosen for OSC analysis, while IL59/DB-5MS was chosen for nitrogen compounds, as each stationary phase set provided the best chromatographic efficiency for these two classes of compounds, respectively. Most compounds were tentatively identified by Lee and Van den Dool and Kratz retention indexes, and spectra-matching to library. Whenever available, compounds were also positively identified via injection of authentic standards.


Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Líquidos Iônicos/química , Compostos de Nitrogênio/análise , Petróleo , Compostos de Enxofre/análise , Brasil , Cromatografia Gasosa-Espectrometria de Massas/normas , Hidrocarbonetos Aromáticos/análise , Hidrocarbonetos Aromáticos/química , Compostos de Nitrogênio/química , Padrões de Referência , Compostos de Enxofre/química
9.
J Chromatogr A ; 1460: 135-46, 2016 Aug 19.
Artigo em Inglês | MEDLINE | ID: mdl-27432785

RESUMO

Insight in the composition of the algae derived bio-oils is crucial for the development of efficient conversion processes and better upgrading strategies for microalgae. Comprehensive two-dimensional gas chromatography (GC×GC) coupled to nitrogen chemiluminescence detector (NCD) and time-of-flight mass spectrometer (TOF-MS) allows to obtain the detailed quantitative composition of the nitrogen containing compounds in the aqueous and the organic fraction of fast pyrolysis bio-oils from microalgae. Normal phase (apolar×mid-polar) and reverse phase column (polar×apolar) combination are investigated to optimize the separation of the detected nitrogen containing compounds. The reverse phase column combination gives the most detailed information in terms of the nitrogen containing compounds. The combined information from the GC×GC-TOF-MS (qualitative) and GC×GC-NCD (quantitative) with the use of a well-chosen internal standard, i.e. caprolactam, enables the identification and quantification of nitrogen containing compounds belonging to 13 different classes: amines, imidazoles, amides, imides, nitriles, pyrazines, pyridines, indoles, pyrazoles, pyrimidines, quinolines, pyrimidinediones and other nitrogen containing compounds which were not assigned to a specific class. The aqueous fraction mostly consists of amines (4.0wt%) and imidazoles (2.8wt%) corresponding to approximately 80wt% of the total identified nitrogen containing compounds. On the other hand, the organic fraction shows a more diverse distribution of nitrogen containing compounds with the majority of the compounds quantified as amides (3.0wt%), indoles (2.0wt%), amines (1.7wt%) and imides (1.3wt%) corresponding to approximately 65wt% of the total identified nitrogen containing compounds.


Assuntos
Cromatografia Gasosa-Espectrometria de Massas , Microalgas/química , Compostos de Nitrogênio/análise , Óleos de Plantas/química , Aminas/análise , Aminas/química , Cromatografia de Fase Reversa , Medições Luminescentes , Microalgas/metabolismo , Compostos de Nitrogênio/química , Óleos de Plantas/metabolismo
10.
J Biosci Bioeng ; 122(1): 70-8, 2016 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-26777234

RESUMO

The relationship between the protein composition of rice and nitrogen compounds (amino acids and oligo-peptides) in the produced sake were investigated using endosperm protein mutant rice (LGC-1, LGC-Jun, Kx433, QA28), sake rice (Yamadanishiki) and cooking rice (Nipponbare, Nihonmasari, Koshihikari). The total nitrogen concentration, amino acid concentration and most peptide peak areas determined by RP-HPLC and gel filtration chromatography of the produced sake were lower when sake was made from a low glutelin content rice mutant compared with other rice varieties. The concentration of nitrogen compounds in the sake positively correlated with the glutelin content of the highly milled rice grains used for sake production. Sake produced using a low glutelin content rice mutant is generally evaluated as having a light taste. Our findings suggest that nitrogen compounds (oligo-peptides and amino acids) derived from rice glutelin significantly contribute to the taste of sake.


Assuntos
Bebidas Alcoólicas/análise , Oryza/química , Proteínas de Plantas/química , Aminoácidos/análise , Culinária , Glutens/análise , Mutação , Nitrogênio/análise , Compostos de Nitrogênio/análise , Oryza/classificação , Oryza/genética , Peptídeos/análise , Paladar
11.
Rapid Commun Mass Spectrom ; 29(8): 735-44, 2015 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-26406488

RESUMO

RATIONALE: Approximately 1 billion m(3) of oil sands process-affected water (OSPW) is currently stored in tailings ponds in Northern Alberta, Canada. The dissolved organic compounds in OSPW have been termed a supercomplex mixture of bitumen-derived substances and continuing efforts to understand its underlying chemical composition are important for evaluating its environmental hazards. METHODS: Packed column supercritical fluid chromatography (SFC) was applied to OSPW analysis for the first time. By combining four columns in series (each 25 cm × 4.6 mm I.D., 5.0 µm bare silica) approximately 80,000 plates were achieved on a 1 m column. Using a simple fixed restrictor, the SFC eluent was coupled directly to ultrahigh-resolution orbitrap mass spectrometry (SFC/Orbitrap-MS). RESULTS: SFC/Orbitrap-MS, with positive and negative atmospheric pressure chemical ionization (APCI +/-), revealed the partial or full chromatographic separation of isomers for a wide array of chemical species, including naphthenic acids (Cn H2n + Z O2 ) and unknown sulfur- and nitrogen-containing molecules. For smaller compounds (e.g. naphthenic acids where n ≤10), or for larger structurally constrained compounds (e.g. C16 naphthenic acid with 9 double-bond equivalents), apparent baseline resolution of many isomers was possible. Isomer-specific MS/MS experiments furthermore allowed characterization of functional groups in novel species. For example, in APCI+ mode, up to 16 isomers of C6 H11 ON were revealed to have amide and amino functionalities. CONCLUSIONS: This combination of high efficiency chromatography and ultra-high mass resolution detection resulted in a powerful method with capabilities for characterizing or 'fingerprinting' unknown species with little interference. The method has great promise for environmental monitoring and forensics in the oil sands region, as well as for further studies on the composition of dissolved organic compounds in OSPW.


Assuntos
Ácidos Carboxílicos/análise , Compostos de Nitrogênio/análise , Campos de Petróleo e Gás/química , Compostos de Enxofre/análise , Poluentes Químicos da Água/análise , Água/análise , Cromatografia com Fluido Supercrítico/métodos , Monitoramento Ambiental/métodos , Espectrometria de Massas/métodos
12.
Ann Occup Hyg ; 59(8): 1074-84, 2015 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-26155991

RESUMO

INTRODUCTION: Chlorination is a method commonly used to keep indoor swimming pool water free from pathogens. However, chlorination of swimming pools produces several potentially hazardous by-products as the chlorine reacts with nitrogen containing organic matter. Up till now, exposure assessments in indoor swimming pools have relied on stationary measurements at the poolside, used as a proxy for personal exposure. However, measurements at fixed locations are known to differ from personal exposure. METHODS: Eight public swimming pool facilities in four Swedish cities were included in this survey. Personal and stationary sampling was performed during day or evening shift. Samplers were placed at different fixed positions around the pool facilities, at ~1.5 m above the floor level and 0-1 m from the poolside. In total, 52 personal and 110 stationary samples of trichloramine and 51 personal and 109 stationary samples of trihalomethanes, were collected. RESULTS: The average concentration of trichloramine for personal sampling was 71 µg m(-3), ranging from 1 to 240 µg m(-3) and for stationary samples 179 µg m(-3), ranging from 1 to 640 µg m(-3). The air concentrations of chloroform were well below the occupational exposure limit (OEL). For the linear regression analysis and prediction of personal exposure to trichloramine from stationary sampling, only data from personal that spent >50% of their workday in the pool area were included. The linear regression analysis showed a correlation coefficient (r2) of 0.693 and a significant regression coefficient ß of 0.621; (95% CI = 0.329-0.912, P = 0.001). CONCLUSION: The trichloramine exposure levels determined in this study were well below the recommended air concentration level of 500 µg m(-3); a WHO reference value based on stationary sampling. Our regression data suggest a relation between personal exposure and area sampling of 1:2, implying an OEL of 250 µg m(-3) based on personal sampling.


Assuntos
Poluição do Ar em Ambientes Fechados/análise , Cloretos/análise , Monitoramento Ambiental/métodos , Compostos de Nitrogênio/análise , Exposição Ocupacional/análise , Piscinas , Trialometanos/análise , Poluentes Atmosféricos/análise , Poluição do Ar em Ambientes Fechados/prevenção & controle , Cloretos/efeitos adversos , Humanos , Modelos Lineares , Compostos de Nitrogênio/efeitos adversos , Exposição Ocupacional/prevenção & controle , Suécia , Trialometanos/efeitos adversos
13.
Environ Sci Technol ; 49(11): 6466-73, 2015 Jun 02.
Artigo em Inglês | MEDLINE | ID: mdl-25961672

RESUMO

The reconstruction of disturbed landscapes back to working ecosystems is an issue of increasing importance for the oil sand areas in Alberta, Canada. In this context, the fate of oil-sand-derived organic material in the tailings sands used for reclamation is of utmost environmental importance. Here we use electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry of maltene fractions to identify compositional variations over a complete oil sand mining and recultivation process chain. On the basis of bulk compound class distributions and percentages of unique elemental compositions, we identify specific compositional features that are related to the different steps of the process chain. The double bond equivalent and carbon number distributions of the N1 and S1O2 classes are almost invariant along the process chain, despite a significant decrease in overall abundance. We thus suggest that these oil-sand-derived components can be used as sensitive tracers of residual bitumen, even in soils from relatively old reclamation sites. The patterns of the O2, O3, and O4 classes may be applied to assess process-chain-related changes in organic matter composition, including the formation of plant-derived soil organic matter on the reclamation sites. The N1O2 species appear to be related to unidentified processes in the tailings ponds but do not represent products of aerobic biodegradation of pyrrolic nitrogen compounds.


Assuntos
Espectrometria de Massas/métodos , Campos de Petróleo e Gás , Poluentes do Solo/análise , Alberta , Biodegradação Ambiental , Ecossistema , Análise de Fourier , Hidrocarbonetos , Compostos de Nitrogênio/análise , Solo/química
14.
J Chromatogr A ; 1373: 159-68, 2014 Dec 19.
Artigo em Inglês | MEDLINE | ID: mdl-25464993

RESUMO

Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/TOFMS) has shown great skill in analyzing complex mixtures such as fossil fuels, especially for compounds at low concentrations. The analysis of N-polyaromatic compounds (NPAC) in coal and crude oil is a great challenge for analytical chemistry due to its environmental and technological importance, and also its diversity of concentration in the matrix. This study is the first report in the applicability of GC×GC/TOFMS for detection of NPAC in a coal tar sample with no fractionation. Normally these compounds are analyzed after sample treatment, making the process expensive and time consuming. However, the higher separation power of GC×GC/TOFMS, compared to 1D-GC, produces cleaner mass spectra in complex samples, which helps in identification of analytes with no pre-fractionation. In this paper, the main objectives were to demonstrate the applicability of GC×GC/TOFMS in the speciation and separation between basic and neutral NPAC from coal tar sample derived from fast pyrolysis, without prior sample fractionation. The methodology used here consisted of chromatographic injection of the diluted sample using a conventional columns set and data analysis by ChromaTOF/Excel™ software. Some basic compounds (pyridines and quinolines) and neutral ones (carbazoles and indoles) were detected with good chromatographic separation and spectral similarity. Tools like spectral deconvolution, extracted ion chromatogram (EIC) and dispersion graphics allowed greater security on the identification and separation of NPAC in this complex sample of coal tar, with no pre-treatment.


Assuntos
Alcatrão/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Compostos de Nitrogênio/análise
15.
Environ Sci Pollut Res Int ; 21(17): 10270-8, 2014 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-24792983

RESUMO

The fate of excess nitrogen in estuaries is determined by the microbial-driven nitrogen cycle, being denitrification a key process since it definitely removes fixed nitrogen as N2. However, estuaries receive and retain metals, which may negatively affect this process efficiency. In this study, we evaluated the role of salt marsh plants in mediating cadmium (Cd) impact on microbial denitrification process. Juncus maritimus and Phragmites australis from an estuary were collected together with the sediment involving their roots, each placed in vessels and maintained in a greenhouse, exposed to natural light, with tides simulation. Similar non-vegetated sediment vessels were prepared. After 3 weeks of accommodation, nine vessels (three per plant species plus three non-vegetated) were doped with 20 mg/L Cd(2+) saline solution, nine vessels were doped with 2 mg/L Cd(2+) saline solution and nine vessels were left undoped. After 10 weeks, vessels were dissembled and denitrification potential was measured in sediment slurries. Results revealed that the addition of Cd did not cause an effect on the denitrification process in non-vegetated sediment but had a clear stimulation in colonized ones (39 % for P. australis and 36 % for J. maritimus). In addition, this increase on denitrification rates was followed by a decrease on N2O emissions and on N2O/N2 ratios in both J. maritimus and P. australis sediments, increasing the efficiency of the N2O step of denitrification pathway. Therefore, our results suggested that the presence of salt marsh plants functioned as key mediators on the degree of Cd impact on microbial denitrification.


Assuntos
Cádmio/toxicidade , Desnitrificação/efeitos dos fármacos , Estuários , Poaceae/metabolismo , Áreas Alagadas , Cádmio/análise , Cádmio/metabolismo , Sedimentos Geológicos/análise , Magnoliopsida/metabolismo , Nitrogênio/análise , Compostos de Nitrogênio/análise , Raízes de Plantas/metabolismo , Plantas , Portugal , Cloreto de Sódio/metabolismo
16.
J Chromatogr A ; 1307: 180-90, 2013 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-23932026

RESUMO

A dual-channel gas chromatographic method is described in this paper that can be conveniently used for quantitation of NF3/CF4 mixtures with a thermal conductivity detector (TCD) on one channel for the quantitation of high-concentrations, and a pulsed discharge helium ionization detector (PDHID) on a second channel for the quantitation of low concentrations. It is shown that adequate separation is achieved on both channels with this dual single-column setup in which column switching as used for NF3/CF4 analysis in industrial chromatographic methods are not required, thus yielding an effective analysis method for laboratory-scale investigations. In addition, the use of packed columns with purified divinylbenzene-styrene co-polymers as the sole stationary phase yields satisfactory resolution between NF3 and CF4 at isothermal conditions of 30°C, with elution times of less than 8min on the TCD channel and less than 4min on the PDHID channel. Consequently, this method allows for reliable, straight-forward quantitation of NF3/CF4 mixtures, which is necessary when studying the commercially important problem of NF3 and CF4 separation by different methods. Therefore, the applicability of the method to studying membrane separation of NF3 and CF4 is briefly discussed and illustrated, for which the dual-channel setup is especially beneficial.


Assuntos
Cromatografia Gasosa/métodos , Fluoretos/análise , Hélio/química , Hidrocarbonetos Fluorados/análise , Compostos de Nitrogênio/análise , Desenho de Equipamento , Fluoretos/química , Fluoretos/isolamento & purificação , Hidrocarbonetos Fluorados/química , Hidrocarbonetos Fluorados/isolamento & purificação , Compostos de Nitrogênio/química , Compostos de Nitrogênio/isolamento & purificação , Reprodutibilidade dos Testes , Temperatura
17.
Environ Pollut ; 183: 175-83, 2013 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-23399401

RESUMO

We determined eleven PAHs and four NPAHs in particulates and regulated pollutants (CO, CO2, HC, NOx, PM) exhausted from motorcycles to figure out the characteristics of motorcycle exhausts. Fluoranthene and pyrene accounted for more than 50% of the total detected PAHs. Among four detected NPAHs, 6-nitrochrysene and 7-nitrobenz[a]anthracene were the predominant NPAHs and were highly correlated relationship with their parent PAHs (R = 0.93 and 0.97, respectively). The PM and HC emissions tended to be close to the PAH emissions. NOx and NPAHs were negatively correlated. Despite their small engine size, motorcycles emitted much more PM and PAHs, showed stronger PAH-related carcinogenicity and indirect-acting mutagenicity, but weaker NPAH-related direct-acting mutagenic potency than automobiles. This is the first study to analyze both PAHs and NPAHs emitted by motorcycles, which could provide useful information to design the emission regulations and standards for motorcycles such as PM.


Assuntos
Motocicletas , Compostos de Nitrogênio/análise , Material Particulado/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Emissões de Veículos/análise , Monitoramento Ambiental , Mutagênicos/análise
18.
Anal Bioanal Chem ; 405(22): 7071-82, 2013 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-23354580

RESUMO

In this study, the chemical composition of sidestream smoke (SSS) emissions of cigarettes are characterised using a laser-based single-photon ionisation time-of-flight mass spectrometer. SSS is generated from various cigarette types (2R4F research cigarette; Burley, Oriental and Virginia single-tobacco-type cigarettes) smoked on a single-port smoking machine and collected using a so-called fishtail chimney device. Using this setup, a puff-resolved quantification of several SSS components was performed. Investigations of the dynamics of SSS emissions show that concentration profiles of various substances can be categorised into several groups, either depending on the occurrence of a puff or uninfluenced by the changes in the burning zone during puffing. The SSS emissions occurring directly after a puff strongly resemble the composition of mainstream smoke (MSS). In the smouldering phase, clear differences between MSS and SSS are observed. The changed chemical profiles of SSS and MSS might be also of importance on environmental tobacco smoke which is largely determined by SSS. Additionally, the chemical composition of the SSS is strongly affected by the tobacco type. Hence, the higher nitrogen content of Burley tobacco leads to the detection of increased amounts of nitrogen-containing substances in SSS.


Assuntos
Monitoramento Ambiental/instrumentação , Espectrometria de Massas/instrumentação , Nicotiana/química , Poluição por Fumaça de Tabaco/análise , Desenho de Equipamento , Compostos de Nitrogênio/análise , Análise de Componente Principal
19.
Water Sci Technol ; 66(3): 666-72, 2012.
Artigo em Inglês | MEDLINE | ID: mdl-22744700

RESUMO

This paper presents results of analyses of water in the river Mala Panew in South West Poland flowing through a rural area with some chemical industry developed. The aims of the work were to investigate the pollutants level in the river, compare the obtained results with obligatory drinking water standards and determine possible health effects when using the river as a source for drinking water production. Attention was given to nitrogen compounds as nitrate(V) ions (NO(3-)) and nitrite(III) ions (NO(2-)), mostly of anthropogenic origin, were detected in the monitored water. The average concentrations of NO(3-) and NO(2-) were 3.54 and 0.286 mg/dm(3), respectively. The chances for non-carcinogenic effects, namely methemoglobinemia, resulting from possible exposure to the examined chemicals were determined based on the analytical and toxicological data. As infants are the sub-population most susceptible to nitrate-induced methemoglobinemia, the assessment was limited to children aged 0-3 years. The determined values expressed by hazard quotient (HQ) and hazard index (HI) indicate that the water pollutants and their concentrations do not exceed unity; however, in the case of infants, the other nitrate sources should be controlled.


Assuntos
Substâncias Perigosas/análise , Compostos de Nitrogênio/análise , Medição de Risco/métodos , Poluentes Químicos da Água/análise , Bebidas , Criança , Água Potável/química , Exposição Ambiental/análise , Alimentos , Geografia , Humanos , Nitratos/análise , Nitratos/toxicidade , Nitritos/toxicidade , Polônia , Rios/química , Incerteza
20.
Environ Sci Pollut Res Int ; 19(8): 3257-67, 2012 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-22374190

RESUMO

PURPOSE: In the reservoir created in the reclaimed land in Isahaya Bay, Japan, Microcystis aeruginosa, which produces microcystins (MCs), bloomed every year, and the water with high levels of MCs in the reservoir has been often drained to Isahaya Bay to adjust the water level. The principal aims of this study are to clarify the water conditions suitable for blooming of M. aeruginosa in the reservoir, to follow the amount of distribution of MCs inside and outside the reservoir, and to discuss how blooming of M. aeruginosa is controlled in the reservoir and how MCs produced by Microcystis spread or accumulate in the aquatic environment. METHOD: We monitored the water quality (temperature, salinity, dissolved inorganic nitrogen (DIN), and dissolved inorganic phosphorus) in the reservoir with seasonal blooming of microalgae including phytoplankton and M. aeruginosa using the concentrations of chlorophyll α and MCs, respectively, and collected the surface sediment in the reservoir and the bay to determine the MC content using the ELISA method. RESULT: M. aeruginosa bloomed in extremely low DIN conditions of the water in warm seasons (spring and late summer to autumn). The year-mean standing stock of MCs was approximately 34.5 kg in the water and 8.4 kg in the surface sediment in the reservoir. Approximately 64.5 kg of MCs was discharged with the effluent to the bay in a year. CONCLUSION: Since a large amount of MCs always suspends in the water in the reservoir and it has been discharged to the bay, suspension-feeding animals are exposed most seriously to the high levels of MCs occurring in these areas. We need to pay attention to the danger of widespread dispersal of MCs and biological concentration of MCs by fish and clam inside and outside the reservoir.


Assuntos
Carcinógenos/metabolismo , Microcistinas/metabolismo , Microcystis/fisiologia , Baías/química , Baías/microbiologia , Carcinógenos/análise , Clorofila/análise , Eutrofização , Sedimentos Geológicos/microbiologia , Japão , Microcistinas/análise , Microcystis/metabolismo , Compostos de Nitrogênio/análise , Compostos de Fósforo/análise , Salinidade , Qualidade da Água
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