Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 42
Filtrar
Mais filtros

País/Região como assunto
Tipo de documento
País de afiliação
Intervalo de ano de publicação
1.
Environ Toxicol ; 35(5): 553-560, 2020 May.
Artigo em Inglês | MEDLINE | ID: mdl-31846182

RESUMO

Arsenic (As) can contaminate air, soil, water, and organisms through mobilization of natural mineralogical deposits or anthropogenic actions. Inorganic-As compounds are more toxic and widely available in aquatic environments, including drinking water reservoir catchments. Since little is known about its effects on prepubertal mammals, the present study focused on it. Hence, As was administered through drinking water to male Wistar rats from postnatal day 23 to 53. Negative control group received vehicle only (filtered water); As 1 group received AsNaO2 at 0.01 mg L-1 and As2 group received AsNaO2 at 10 mg L-1 . It was investigated hepatic and renal toxicity of AsNaO2 (ie, histopathology and apoptosis analysis), as well as its mutagenicity (ie, micronucleus test in liver and bone marrow), cytotoxicity (ie, frequency and type of erythrocytes in blood), and genotoxicity (ie, comet assay in blood). Also, As determination was performed in hepatic and renal tissues. Data obtained revealed that immature organisms present a pattern of arsenic accumulation similar to that observed in adults, suggesting similarity in metabolic processes. In addition, liver showed to be an important target tissue for As toxicity in these experimental conditions, exhibiting infiltrate of defense cells, DNA damages, and increased apoptosis rates.


Assuntos
Envelhecimento/efeitos dos fármacos , Arsenitos/toxicidade , Doença Hepática Induzida por Substâncias e Drogas/etiologia , Dano ao DNA , Poluentes Ambientais/toxicidade , Micronúcleos com Defeito Cromossômico/induzido quimicamente , Compostos de Sódio/toxicidade , Envelhecimento/genética , Animais , Doença Hepática Induzida por Substâncias e Drogas/genética , Ensaio Cometa , Relação Dose-Resposta a Droga , Masculino , Testes para Micronúcleos , Ratos , Ratos Wistar
2.
Anal Bioanal Chem ; 408(17): 4547-66, 2016 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-27020927

RESUMO

Interest in the determination of elemental impurities in pharmaceuticals has increased in recent years because of changes in regulatory requirements and the need for changing or updating the current limit tests recommended in pharmacopeias. Inductively coupled plasma (ICP) optical emission spectrometry and ICP mass spectrometry are suitable alternatives to perform multielemental analysis for this purpose. The main advantages and limitations of these techniques are described, covering the applications reported in the literature in the last 10 years mainly for active pharmaceutical ingredients, raw materials, and pharmaceutical dosage forms. Strategies used for sample preparation, including dissolution in aqueous or organic solvents, extraction, wet digestion and combustion methods are described, as well as direct solid analysis and ICP-based systems applied for speciation analysis. Interferences observed during the analysis of pharmaceutical products using ICP-based methods are discussed. Methods currently recommended by pharmacopeias for elemental impurities are also covered, showing that the use of ICP-based methods could be considered as a trend in the determination of these impurities in pharmaceuticals. However, the development of a general method that is accurate for all elemental impurities and the establishment of an official method are still challenges. In this regard, the main drawbacks and suitable alternatives are discussed.


Assuntos
Espectrometria de Massas/métodos , Preparações Farmacêuticas/química
3.
Anal Chem ; 85(1): 374-80, 2013 Jan 02.
Artigo em Inglês | MEDLINE | ID: mdl-23171470

RESUMO

An effective approach to the digestion of fluoropolymers for the determination of Ag, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, and Ni impurities has been developed using microwave-induced combustion (MIC) in closed quartz vessels pressurized with oxygen. Samples that were examined included the following: polytetrafluorethylene (PTFE); polytetrafluoroethylene with an additional modifier, perfluoropropylvinylether (PTFE-TFM); and fluorinated ethylene propylene (FEP). A quartz device was used as a sample holder, and the influence of the absorber solution was evaluated. Determination of trace elements was performed by inductively coupled plasma-optical emission and mass spectrometry. Neutron activation analysis (NAA) was used for validation purposes. Results were also compared to those obtained using microwave-assisted acid extraction in high-pressure closed systems. Dilute nitric acid (5 mol L(-1)), which was selected as the absorbing medium, was used to reflux the sample for 5 min after the combustion. Using these conditions, agreement for all analytes was better than 98% when compared to values determined by NAA. The residual carbon content in the digests was lower than 1%, illustrating the high efficiency of the method. Up to 8 samples could be digested within 30 min using MIC, providing a suitable throughput, taking into account the inertness of such samples.


Assuntos
Espectrometria de Massas , Micro-Ondas , Politetrafluoretileno/química , Oligoelementos/análise , Nêutrons , Ácido Nítrico/química , Quartzo/química
4.
Anal Chem ; 85(10): 5015-22, 2013 May 21.
Artigo em Inglês | MEDLINE | ID: mdl-23614538

RESUMO

This paper reports, for the first time, the development of an analytical method employing modified matrix solid-phase dispersion (MSPD) for the extraction of CH3Hg(+) and Hg(2+) species from fish samples. Separation and determination of mercury species were performed by gas chromatography coupled to mass spectrometry (GC/MS). Important MSPD parameters, such as sample mass, type and mass of solid support, concentration of extraction solution (HCl and NaCl), and stirring time, were investigated by the response surface methodology. The derivatization step and the separation of mercury species were also evaluated for the determination by GC/MS. Quantitative recoveries were obtained with 0.2 g of fish sample, 0.5 g of SiO2 as the solid support, 0.5 mol L(-1) NaCl and 4.2 mol L(-1) HCl as the extraction solution, and 1 min stirring time. The MSPD method showed to be suitable for the extraction and determination of mercury species in certified reference materials of dogfish liver (DOLT-3) and dogfish muscle (DORM-2). It had good agreement (about 99%) with the certified values, and the relative standard deviation was lower than 9.5%. The limits of detection were 0.06 and 0.12 µg g(-1), for CH3Hg(+) and Hg(2+), respectively. A matrix effect was observed, and the quantification was carried out by the matrix-matched calibration. The method was applied to tuna fish ( Thunnus thynnus ), angel shark ( Squatina squatina ), and guitarfish ( Rhinobatos percellens ) samples. The results of the mercury speciation by MPSD and GC/MS were compared to the total mercury concentration determined by flow injection cold vapor generation inductively coupled plasma mass spectrometry, after microwave-assisted digestion. Agreement ranged from 102% to 105%.


Assuntos
Métodos Analíticos de Preparação de Amostras/métodos , Peixes , Mercúrio/análise , Mercúrio/isolamento & purificação , Compostos de Metilmercúrio/análise , Compostos de Metilmercúrio/isolamento & purificação , Extração em Fase Sólida/métodos , Animais , Contaminação de Alimentos/análise , Cromatografia Gasosa-Espectrometria de Massas , Limite de Detecção
5.
Anal Bioanal Chem ; 405(24): 7615-42, 2013 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-23780223

RESUMO

Fluorine, chlorine, bromine, and iodine have been studied in biological samples and other related matrices owing to the need to understand the biochemical effects in living organisms. In this review, the works published in last 20 years are covered, and the main topics related to sample preparation methods and analytical techniques commonly used for fluorine, chlorine, bromine, and iodine determination in biological samples, food, drugs, and plants used as food or with medical applications are discussed. The commonest sample preparation methods, as extraction and decomposition using combustion and pyrohydrolysis, are reviewed, as well as spectrometric and electroanalytical techniques, spectrophotometry, total reflection X-ray fluorescence, neutron activation analysis, and separation systems using chromatography and electrophoresis. On this aspect, the main analytical challenges and drawbacks are highlighted. A discussion related to the availability of certified reference materials for evaluation of accuracy is also included, as well as a discussion of the official methods used as references for the determination of halogens in the samples covered in this review.


Assuntos
Bioensaio/normas , Química Analítica/normas , Halogênios/análise , Animais , Bioensaio/tendências , Halogênios/química , Humanos
6.
J Sep Sci ; 36(20): 3411-8, 2013 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-23946243

RESUMO

This work reports the development of a dispersive liquid-liquid microextraction method for the simultaneous extraction, preconcentration, and derivatization of Hg(2+) and CH3Hg(+) species from water samples for further determination by GC-MS. Some parameters of the proposed method, such as volume and type of disperser and extraction solvent, and Na[B(C6H5)4] concentration were investigated using response surface methodology. Suitable recoveries were obtained using 80 µL C2 Cl4 (as extraction solvent), 1000 µL ethanol (as disperser solvent), and 300 µL 2.1 mmol/L Na[B(C6H5)4] (as derivatizing agent). Accuracy was evaluated in terms of recovery and ranged from 87 to 99% with RSD values <7%. In addition, a certified reference material of water (NIST 1641d) was analyzed and agreed with the certified value about 107% (for Hg(2+)), with RSD values <8.5%. LODs were 0.3 and 0.2 µg/L, with enrichment factors of 112 and 115 for Hg(2+) and CH3Hg(+), respectively. The optimized method was applied for the determination of Hg(2+) and CH3Hg(+) in tap, well, and lake water samples.


Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Microextração em Fase Líquida/métodos , Compostos de Mercúrio/análise , Compostos de Mercúrio/isolamento & purificação , Compostos de Metilmercúrio/análise , Compostos de Metilmercúrio/isolamento & purificação , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificação , Água Doce/química
7.
Food Chem ; 429: 136916, 2023 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-37481982

RESUMO

This work presents the first report of the application of microwave-induced combustion in disposable vessels (MIC-DV) as a simple and fast sample preparation step for fluoride determination by ion-selective electrode (ISE) in leguminous seeds and oilseeds samples. Several experimental conditions of MIC-DV were evaluated, such as sample mass, absorbing solution, volume of combustion igniter, purging time with oxygen, and the use of successive combustion cycles. The accuracy of MIC-DV/ISE method was evaluated by comparing the results obtained by microwave-induced combustion and determination by ion chromatography, with agreements ranged from 94 to 106%. The method allowed to achieve relatively low limits of quantification (8.3 to 16 µg g-1) comparing to AOAC method (40 µg g-1), besides the use of small amounts of reagents, less handling of digests, making the method greener and with portable features comparing to other methods.


Assuntos
Fabaceae , Flúor , Eletrodos Seletivos de Íons , Sementes , Micro-Ondas
8.
Anal Chim Acta ; 1273: 341536, 2023 Sep 08.
Artigo em Inglês | MEDLINE | ID: mdl-37423667

RESUMO

A simple, fast and promising sample preparation method based on microwave-induced combustion in disposable vessels (MIC-DV) was developed for Cl and S determination in crude oil by inductively coupled plasma optical emission spectrometry (ICP-OES). The MIC-DV consists of a new approach of conventional microwave-induced combustion (MIC). For the combustion, crude oil was pipetted on a disk of filter paper and placed on a quartz holder, followed by the addition of igniter solution (40 µL of 10 mol L-1 NH4NO3). The quartz holder was inserted into a commercial 50 mL disposable polypropylene vessel containing the absorbing solution, which was then inserted in an aluminium rotor. The combustion occurs under atmospheric pressure in a domestic microwave oven not compromising the operator's safety. The following parameters of combustion were evaluated: type, concentration and volume of absorbing solution, sample mass and the possibility of performing consecutive combustion cycles. Using MIC-DV, up to 10 mg of crude oil were efficiently digested, using 2.5 mL of ultrapure H2O as absorbing solution. Moreover, up to 5 consecutive combustion cycles were possible without analyte losses, reaching a total sample mass of 50 mg. The MIC-DV method was validated according to Eurachem Guide recommendations. Results obtained for Cl and S by MIC-DV were in agreement with those obtained using conventional MIC, as well as those obtained for S in a certified reference material of crude oil (NIST 2721). Analyte spike recovery experiments were performed and recoveries at three concentration levels ranged from 99 to 101% for Cl and from 95 to 97% for S, indicating a good accuracy. The limit of quantification achieved by ICP-OES after MIC-DV were 73 and 50 µg g-1 for Cl and S respectively, applying 5 consecutive combustion cycles.

9.
Environ Sci Pollut Res Int ; 30(3): 6068-6079, 2023 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-35986114

RESUMO

The production of sustainable catalytic supports for palladium nanoparticles is always desired, even more so through the recovery of biomass residues. In this sense, two different solids were investigated - chitosan/cellulose film and corn stem biochar - as catalytic supports of palladium nanoparticles. The solids were carefully characterized and tested in the Suzuki-Miyaura reaction, a typical cross-coupling reaction. The developed catalytic systems proved to be efficient and sustainable, promoted the formation of target products very well, and demanded green reactants under environmentally appropriate conditions. With the results shown in the manuscript, it is expected to contribute to the valorization of biomass and agro-industrial residues in the development of new catalysts for the chemical industry.


Assuntos
Quitosana , Nanopartículas Metálicas , Nanopartículas Metálicas/química , Paládio/química , Quitosana/química , Zea mays , Celulose/química , Catálise
10.
Anal Chim Acta ; 1199: 339569, 2022 Mar 22.
Artigo em Inglês | MEDLINE | ID: mdl-35227390

RESUMO

In this work, high purity graphite, a high chemically stable material, was effectively digested using a single method allowing compatible solutions for the further multitechnique determination of halogens by: ion chromatography (F and Cl), inductively coupled plasma mass spectrometry (Cl, Br and I) and by ion selective electrode (only for F). The recent system using microwave-induced self-ignition (MISI) is based on the strong interaction between microwave radiation and graphite in a closed system pressurized with oxygen (Maxwell-Wagner effect). Carbon-based materials present intense and specific interfacial polarization when exposed to microwave electromagnetic field resulting in a fast heating rate. This effect associated to a pressurized oxygen system, provides a quick self-ignition of carbon-based materials and consequent combustion/digestion of organic matrices. Under optimized conditions, sample masses up to 600 mg were fully digested in a quartz vessel under 20 bar of oxygen pressure and using just a diluted solution (100 mmol L-1 NH4OH) for the quantitative absorption of all the analytes. MISI method was validated, and the accuracy (better than 94%) was evaluated by comparison of results obtained by pyrohydrolysis for two coal certified reference materials as well as with subsequent analytes determination by the three techniques: IC, ICP-MS and ISE. It is important to point out that no filter paper disks, electrical connections or other ignition aids are required as in the case of previous or classical combustion methods. Moreover, just a diluted absorbing solution was used resulting in negligible blanks and relatively low limits of detection. The digestion efficiency was higher than 99%, making the proposed method a suitable and powerful alternative for the quasi complete digestion of graphite and determination of halogens virtually free of interferences.


Assuntos
Grafite , Halogênios , Digestão , Halogênios/análise , Espectrometria de Massas/métodos , Micro-Ondas
11.
Chemosphere ; 301: 134661, 2022 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-35452647

RESUMO

High amounts of phosphogypsum (PG) are generated in the production of phosphoric acid. Previous literature demonstrates that obtaining rare earth elements (REE) from PG is a promising alternative to managing this waste. However, the reported leaching efficiencies are low in most cases, or drastic leaching conditions are required. Therefore, this work aimed to study the leaching conditions of REE from PG to obtain high leaching efficiency values. Initially, a 24 factorial experimental design investigated the factors that affect the conventional acid leaching of REE from PG (leaching acid (citric and sulfuric acid), solid/liquid ratio, acid concentration, and temperature). Better leaching efficiency values of the sum of all REE (62.0% and 89.7% for citric and sulfuric acid, respectively) were obtained using an acid concentration of 3 mol L-1, solid/liquid ratio of 1/20 g mL-1, and temperature of 80 °C. Subsequently, the experiments optimization, performed through a central composite rotational design, indicated that the maximum leaching efficiency was achieved using a sulfuric acid concentration of 2.9 mol L-1, solid/liquid ratio of 1.7/20 g mL-1, and 55 °C. Under these conditions, the leaching efficiency of the sum of all REE was 90.0%. Leaching kinetics results showed that the equilibrium was reached in about 20 min for most REE. The mechanism investigation suggested that surface chemical reaction and diffusion through the boundary layer controlled the leaching.


Assuntos
Metais Terras Raras , Ácidos , Sulfato de Cálcio , Fósforo , Temperatura
12.
Food Chem ; 344: 128671, 2021 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-33261997

RESUMO

Direct analysis of flour was proposed for the determination of Cl and S by an elemental analyzer for the first time. The main operational conditions of the direct solid sampling elemental analysis (DSS-EA) were optimized and calibrated by standard solutions, rather than by certified reference material (CRM). Accuracy was evaluated by the analysis of CRM of rice flour and by comparison with analyte determination by independent techniques, i.e., ion chromatography and inductively coupled plasma optical emission spectrometry; both were carried out after microwave-induced combustion. Sample mass from 0.5 to 260 mg was used and limits of quantification of 1.2 µg g-1 for Cl and 0.2 µg g-1 for S were achieved. Wheat, whole wheat, potato and corn flour were analyzed by DSS-EA. Concentrations of Cl and S ranged from 4.8 to 685 µg g-1 and from 13 to 1328 µg g-1, respectively.


Assuntos
Cloro/análise , Farinha/análise , Análise de Alimentos/métodos , Enxofre/análise , Calibragem , Micro-Ondas , Oryza/química , Triticum/química
13.
Talanta ; 226: 122157, 2021 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-33676704

RESUMO

In this work, two microwave-assisted sample preparation methods based on combustion and ultraviolet digestion for futher determination of Br, Cl, and I in blood by inductively coupled plasma mass spectrometry were proposed. For microwave-induced combustion (MIC), blood was spotted on square pieces of Munktell TFN paper, and water and diluted NH4OH were evaluated as absorbing solutions. The stability of the analytes in the spotted blood was also evaluated. During 90 days, no changes of halogen content were observed for samples (with and without anticoagulant) on paper stored in a desiccator at 20 ± 5 °C. Whole blood was also digested by microwave-assisted ultraviolet digestion (MAD-UV). Some parameters as the volume of HNO3 solution, the influence of H2O2, and the effect of UV radiation were investigated. The interferences caused by C and K on halogen determination were carefully investigated. The results for MIC and MAD-UV and Br, Cl and I determination by ICP-MS presented no difference. The accuracy of MIC and MAD-UV was also evaluated by analyte spike with reference solutions of Br, Cl and I using inorganic species and also organic I standard (T4-levothyroxine). For both methods, recoveries were 94 and 108% for Br, 96 and 103% for Cl, and 104 and 97% for I. In case of organic I, recoveries were 99 and 111% for MIC and MAD-UV, respectively. The limits of quantification for MIC and MAD-UV after ICP-MS determination were 0.06 and 0.04 µg g-1 for Br, 14 and 30 µg g-1 for Cl and 12 and 8 ng g-1 for I, respectively. The proposed methods provide a suitable digestion approach, assuring safety and high digestion efficiency for further halogen determination in blood, with the possibility to use in clinical analysis.


Assuntos
Halogênios , Micro-Ondas , Peróxido de Hidrogênio , Espectrometria de Massas , Análise Espectral
14.
Food Chem ; 344: 128677, 2021 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-33261993

RESUMO

Microwave-induced combustion (MIC) system for further Cl, Br, and I determination in granola by inductively coupled plasma mass spectrometry (ICP-MS) was proposed. A high sample mass of granola was pressed as pellets and inserted into the proposed MIC system. Water and NH4OH were evaluated as absorbing solutions. The accuracy was estimated by the analysis of two certified reference materials and also by spike recoveries. Using the optimized conditions (zirconium ball milling, 1 g of granola and 6 mL of 50 mmol L-1NH4OH), the agreement with the certified values ranged from 94 to 98% and recoveries higher than 95% were obtained. Low carbon concentration in digests (<25 mg L-1) was achieved, minimizing interferences by ICP-MS. Blanks were negligible and only diluted solutions were required. The concentration in samples ranged from 322 to 896, 0.618 to 0.980 and < 0.002 to 0.181 µg g-1 for Cl, Br and I, respectively.


Assuntos
Análise de Alimentos/métodos , Halogênios/análise , Espectrometria de Massas , Bromo/análise , Cloro/análise , Iodo/análise , Limite de Detecção , Micro-Ondas , Lanches
15.
J Hazard Mater ; 384: 121137, 2020 02 15.
Artigo em Inglês | MEDLINE | ID: mdl-31685318

RESUMO

Ten different adsorbent materials were tested to adsorb indium (III) from leachates of LCD screens, aiming to concentrate this valuable material. Artificial neural network (ANN) and adaptive neuro-fuzzy inference system (ANIFS) were applied to analyze the indium (III) adsorption. The input variables for the network models were: specific surface area, point of zero charge, adsorbent dosage and contact time. Adsorption capacity (q) was used as output variable. The adsorption capacity values ranged from 8.203 to 1000 mg g-1. The ANN modeling presented the best fit when the Levenberg-Marquardt algorithm was used. The ANFIS modeling presented the optimum performance when the hybrid method was used. Among the tested adsorbents, chitosan presented the best performance; attaining adsorption capacity of 1000 mg g-1 within 20 min. This is an excellent value since the maximum indium concentration in LCD screens is 0.613 mg g-1. This high capacity was attributed to the coordination ligation between chitosan and indium (III).

16.
Nutrients ; 12(4)2020 Apr 13.
Artigo em Inglês | MEDLINE | ID: mdl-32295049

RESUMO

Salt iodization is the main public health policy to prevent and control iodine deficiency disorders. The National Salt Iodization Impact Assessment Survey (PNAISAL) was conducted to measure iodine concentration among Brazilian schoolchildren. A survey including 6-14-year-old schoolchildren from public and private schools from all 26 Brazilian states and the Federal District was carried out in the biennia 2008-2009 and 2013-2014. Municipalities, schools, and students were randomly selected. Students were interviewed at school using a standard questionnaire, which included the collection of demographic, educational, weight, height, and 10 mL non-fasting urine collection information. The analyses were weighted according to the population of students per federative unit. The median urinary iodine concentration (MUIC) for the entire sample by region, federative unit per school, and student characteristics, was described from the cutoff points defined by the World Health Organization (severe disability: <20 µg/L, moderate: 20-49 µg/L, mild: 50-99 µg/L, adequate: 100-199 µg/L, more than adequate: 200-299 µg/L, and excessive: >300 µg/L). In total, 18,864 students (95.9% of the total) from 818 schools in 477 municipalities from all federative units were included in this study. Almost 70% were brown skin color, nine-years-old or older, studied in urban schools, and were enrolled in elementary school. The prevalence of overweight/obesity, as measured by body mass index (BMI) for age, was about twice as high compared to nutritional deficits (17.3% versus 9.6%). The MUIC arrived at 276.7 µg/L (25th percentile = 175.5 µg/L and 75th percentile = 399.71 µg/L). In Brazil as a whole, the prevalence of mild, moderate, and severe deficit was 6.9%, 2.6%, and 0.6%, respectively. About one-fifth of the students (20.7%) had adequate iodine concentration, while 24.9% and 44.2% had more than adequate or excessive concentration, respectively. The prevalence of iodine deficits was significantly higher among younger female students from municipal public schools living in rural areas with the lowest BMI. The median urine iodine concentration showed that Brazilian students have an adequate nutritional intake, with a significant proportion of them evidencing overconsumption of this micronutrient.


Assuntos
Fenômenos Fisiológicos da Nutrição do Adolescente/fisiologia , Fenômenos Fisiológicos da Nutrição Infantil/fisiologia , Ingestão de Alimentos , Iodo/administração & dosagem , Iodo/deficiência , Estado Nutricional , Adolescente , Fatores Etários , Biomarcadores/urina , Índice de Massa Corporal , Brasil/epidemiologia , Criança , Estudos Transversais , Feminino , Humanos , Iodo/urina , Masculino , Instituições Acadêmicas , Fatores Sexuais , Inquéritos e Questionários , Fatores de Tempo
17.
Talanta ; 218: 121129, 2020 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-32797886

RESUMO

A new procedure is proposed for the determination of metal contaminants (Cr, Fe, Mg, Mn, Na and Ni) in polymeric diphenylmethane diisocyanate (PMDI), a raw material used to produce polyurethane polymers. The feasibility of using Zeeman-effect background correction graphite furnace atomic absorption spectrometry (GF AAS) and direct sampling (DS) was evaluated. Calibration using aqueous standard solutions was feasible and chemical modifiers as well as reference materials for this purpose were unnecessary. Relatively high sample masses (up to 23 mg) were used allowing very low limits of detection ranging from 0.06 ng g-1 to 1 ng g-1 (Fe and Mg) up to 3  ng g-1 (Ni), with relative standard deviation lower than 15%. The following parameters were evaluated: pyrolysis and atomization temperatures , sample mass, as well as the use of low sensitivity conditions (Zeeman effect background correction magnetic field strength adjustment and the use of a secondary wavelength for Fe and Na determinations, respectively). Results were compared with those obtained by microwave-assisted digestion and microwave-induced combustion with subsequent analytes determination by inductively coupled plasma optical emission spectrometry (ICP-OES) and by inductively coupled plasma mass spectrometry (ICP-MS). No significant difference was observed between the results obtained by DS-GF AAS, ICP-MS and ICP-OES after both digestion systems. The proposed DS-GF AAS method allowed the determination of six elements in PMDI (which is considered as a complex matrix) with limits of detection lower than those achieved by other methods. This new procedure can be used as quality control of polyurethanes industry for ultra-trace inorganic impurities.

18.
Environ Sci Pollut Res Int ; 27(17): 21914-21923, 2020 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-32285391

RESUMO

In this work, some trace elements (As, Cd, Cr, Cu, and Pb) were determined for the first time in the crustacean Sergio mirim (Decapoda: Thalassinidea: Callianassidae) from Southern Coast (Rio Grande, RS) of Brazil. The trace element determination was carried out by graphite furnace atomic absorption spectrometry (GF AAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different microwave radiation-based sample digestion methods were evaluated. The analyte concentration ranged from 1.45 to 3.70 µg g-1 for As, 0.615 to 0.942 µg g-1 for Cd, 0.884 to 7.20 µg g-1 for Cr, 122 to 275 µg g-1 for Cu, and 0.390 to 0.916 µg g-1 for Pb. The limits of quantification for As, Cd, Cr, Cu, and Pb were 0.12, 0.01, 0.16, 0.92, and 0.06 µg g-1, respectively. The accuracy was evaluated by results comparison between GF AAS and ICP-MS techniques, as well as by analysis of certified reference materials of fish muscle and oyster tissue, with agreement from 92 to 108%. The feasibility of using Sergio mirim as a promising environmental bioindicator candidate was evaluated, since that it is an abundant organism in the studied area (South cost of Brazil) as well as in other places around the world.


Assuntos
Decápodes , Oligoelementos/análise , Animais , Brasil , Alimentos Marinhos/análise , Espectrofotometria Atômica
19.
Artigo em Inglês | MEDLINE | ID: mdl-31521749

RESUMO

The aim of this study was to determine whether purinergic signaling is a pathway associated with fumonisin B1 (FB1)-induced impairment of immune and hemostatic responses. We also determined whether dietary supplementation with diphenyl diselenide (Ph2Se2) prevents or reduces these effects. Splenic nucleoside triphosphate diphosphohydrolase (NTPDase) activity for adenosine triphosphate (ATP) and adenosine diphosphate (ADP) as substrates and total blood thrombocytes counts were significant lower in silver catfish fed with FB1-contaminated diets than in fish fed with a basal diet, while splenic adenosine deaminase (ADA) activity and metabolites of nitric oxide (NOx) levels were significant higher. Also, glutathione peroxidase (GPx) and superoxide dismutase (SOD) activities were significant lower in silver catfish fed with FB1-contaminated diets than in fish fed with a basal diet. Dietary supplementation with 3 mg Ph2Se2/kg of feed effectively modulated splenic NTPDase (ATP as substrate), ADA, GPx and SOD activities, as well as NOx levels, and was partially effective in the modulation of spleen NTPDase activity (ADP as substrate) and total blood thrombocytes count. These data suggest that splenic purinergic signaling of silver catfish fed with FB1-contaminated diets generates a pro-inflammatory profile that contributes to impairment of immune and inflammatory responses, via reduction of splenic ATP hydrolysis followed possible ATP accumulation in the extracellular environment. Reduction of ADP hydrolysis associated with possible accumulation in the extracellular environment can be a pathophysiological response that restricts the hemorrhagic process elicited by FB1 intoxication. Supplementation with Ph2Se2 effectively modulated splenic enzymes associated with control of extracellular nucleotides (except ADP; that was partially modulated) and nucleosides, thereby limiting inflammatory and hemorrhagic processes.


Assuntos
Ração Animal/análise , Derivados de Benzeno/farmacologia , Peixes-Gato , Doenças dos Peixes/induzido quimicamente , Fumonisinas/toxicidade , Compostos Organosselênicos/farmacologia , Baço/efeitos dos fármacos , Animais , Plaquetas , Dieta/veterinária , Contaminação de Alimentos , Glutationa Peroxidase/metabolismo , Nitratos/sangue , Nitritos/sangue , Transdução de Sinais , Superóxido Dismutase/metabolismo
20.
Chemosphere ; 258: 127284, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32563913

RESUMO

The exposition of mate (Ilex Paraguariensis A. St.-Hil.) to As and Cd was investigated in plants derived from young mini-cuttings. Mate plants were cultivated in a closed soilless system, composed of coarse sand as substrate and flood fertirrigation. Plantlets were fertirrigated with nutritive solution and As and Cd solutions were added to the nutritive solution in the final concentration of 8 and 17 mg L-1 (As) and of 17 and 33 mg L-1 (Cd) during 14 days. Results show that stem diameter and Dickson quality index (DQI) variables could not be used as a potential indicator of accumulation of As and Cd. The shoot height, number of leaves and chlorophyll index are variables easy and quick to measure and they can be used as parameters to evaluate the stress caused in mate plants cultivation in a closed soilless system. The highest concentration of As and Cd was in roots of plants. Beyond the roots, As and Cd also can be translocated to the leaves achieving high concentrations. In addition, leaves from the treated mate plants were submitted to a hot infusion extraction in order to simulate the traditional beverage and As and Cd were determined in the infusion. Regarding to the infusion procedure, considerable As and Cd amounts were extracted from the leaves leading to conclude that this way of consumption can be an important source of toxic elements for the human diet.


Assuntos
Arsênio/toxicidade , Cádmio/farmacocinética , Contaminação de Alimentos/análise , Ilex paraguariensis/efeitos dos fármacos , Folhas de Planta/química , Cádmio/toxicidade , Exposição Dietética , Poluentes Ambientais/farmacocinética , Poluentes Ambientais/toxicidade , Humanos , Extratos Vegetais/análise , Extratos Vegetais/química , Raízes de Plantas/química , Chás de Ervas , Distribuição Tecidual
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA