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A simple method based on HR-CS FAAS for multi-element determination of Cu, Fe, Mn and Zn in medicinal plants

A simple method to determine Cu, Fe, Mn and Zn in single aliquots of medicinal plants by HR-CS FAAS is proposed. The main lines for Cu, Mn and Zn, and the alternate line measured at the wing of the main line for Fe at 248.327 nm allowed calibration within the 0.025 - 2.0 mg L-1 Cu, 1.0 - 20.0 mg L-1 Fe, 0.05 - 2.0 mg L-1 Mn, 0.025 - 0.75 mg L-1 Zn ranges. Nineteen medicinal plants and two certified plant reference materials were analyzed. Results were in agreement at a 95% confidence level (paired t-test) with reference values. Limits of detection were 0.12 μg L-1 Cu, 330 μg L-1 Fe, 1.42 μg L-1 Mn and 8.12 μg L-1 Zn. Relative standard deviations (n=12) were ≤ 3% for all analytes. Recoveries in the 89 - 105% (Cu), 95 - 108% (Fe), 94 - 107% (Mn), and 93 - 110% (Zn) ranges were obtained.

Desempenho e morfometria duodenal de frangos de corte submetidos a diferentes níveis de energia e programas de alimentação de 42 a 57 dias de idade

This experiment was conducted to evaluate the use of different energy levels and amino acid recommendations on performance, carcass yield and intestinal morphometry of broilers from 42 to 57 days of age. We used 1,600 one-day old male broilers (Cobb 500) in a completely randomized design arranged in a 2x4 factorial scheme with 3,200 and 3,600 kcal ME/kg and four different feed programs. The metabolizable energy levels and the feed programs did not determine significant differences in carcass characteristics for choosing a level of energy or a feed program, thus the energy level and the recommendations of amino acids that determine the highest cost-benefit ratio should prevail. It was observed that 3,600 kcal ME/kg resulted in some improvement on performance and morphometry of the intestinal mucosa, also the fractioning of digestible amino acid requirements during two periods resulted in worse performance and intestinal villi height.

Synthesis, characterization and thermal study of solid mandelate of some bivalent transition metal ions in CO2 and N2 atmospheres

Solid state M-L, where M stands for bivalent transition metals (Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II)) and L is mandelate, were synthesized. Simultaneous thermogravimetry and differential scanning calorimetry, elemental analysis and complexometry were used to establish the stoichiometry and to study the thermal behaviour of these compounds in CO2 and N2 atmospheres. The results show that all the compounds were obtained in the anhydrous state and in agreement with the general formula ML2. The thermal decomposition of the compounds occurs in a single (Cu(II)), two (Ni(II)) three (Fe(II), Co(II)), four (Mn(II)) and five (Zn(II)) steps. The results also provided information concerning the ligand's denticity, thermal behaviour, final residues and identification of gaseous products evolved during the thermal decomposition of these compounds. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Condutividade elétrica da solução nutritiva e acúmulo de macro e micronutrientes no cultivo de crisântemo

The study of growth and uptake of nutrients is important to determine the times of increased demand in order to schedule the fertigation. The present research was developed with the objective of evaluating the effects of different levels of electrical conductivity on growth and accumulation of nutrients in chrysanthemum plants under greenhouse conditions. The electrical conductivity levels on the applied solution were 1.42, 1.65, 1.89, 2.13 and 2.36 dS m-1 (bud vegetative stage); 1.71, 1.97, 2.28, 2.57 and 2.85 dS m-1 (bud stage). The dry mass of the aerial portion of the plant and the contents of macronutrients and micronutrients were determined every 14 days. The nutrient accumulation in chrysanthemum plant showed similar trend as compared to dry matter accumulation. The nutrients presented the following order of absorption: K>N>Ca>Mg>P>S (1425, 892, 184, 150, 110 and 59 mg plant-1) and Fe>Zn>B>Mn>Cu (2254, 2219, 1725, 1287, 210 μg plant-1). The content of most nutrients increased with increase in electrical conductivity of the solution, without salt effect up to EC of 2.85 dS m-1.

Voltammetric determination of ethyl acetate in ethanol fuel using a Fe 3+/Nafion®-coated glassy carbon electrode

A voltammetric method for the determination of ethyl acetate in ethanol fuel using a Fe3+/Nafion®-coated glassy carbon electrode (GCE) is proposed. The ethyl acetate present in the ethanol fuel was previously converted to acetohydroxamic acid via pretreatment with hydroxylamine chloride. The acetohydroxamic acid promptly reacted with the iron (III) present in the film, producing iron (III) acetohydroxamate, which presents a well-defined voltammetric peak current at -0.02 V. Optimization of the voltammetric parameters for the cyclic, linear sweep, square wave, and differential pulse modalities was carried out for this chemically-modified electrode. Square wave voltammetry afforded the best response for acetohydroxamic acid detection. The analytical curve for this species was linear from 9 to 100 μmol L 1 according to the following equation: ip (μA) = 0.27 + 2.55Cacetohydroxamic acid (μmol L 1), with linear correlation coefficient equal to 0.993. The technique presented limit of detection equal to 5.3 μmol L 1 and quantification limit of 17.6 μmol L 1. The proposed method was compared to the official method of ethyl acetate analysis (Gas Chromatography), and a satisfactory correlation was found between these techniques. © 2012 Elsevier Ltd. All rights reserved.

Gas phase photocatalytic bacteria inactivation using metal modified TiO2 catalysts

The present study describes the efficiency of heterogeneous photocatalytic reactor for the inactivation of three air born bacteria, Escherichia coli, Bacillus subtilis and Staphylococcus aureus using metal modified TiO2 photocatalysts and blacklight irradiation. The catalysts were prepared by photodeposition of silver, palladium or iron on commercial TiO2, immobilized on glass plates. X-ray photoelectron spectroscopy analysis was applied to determine the atomic percentage and species of each metal on the TiO2 surface, showing that 85% of silver, 73% of palladium and 45% of iron were present in metallic form on TiO2 surface. The plates were positioned on the inner lateral walls of a chamber through which the contaminated air flow passed for disinfection. Irradiation of bare TiO 2 resulted in 50% inactivation of E. coli while 41% and 35% inactivation of B. subtilis and S. aureus were obtained, respectively. When metal modified TiO2 was applied, the inactivation of B. subtilis was improved to 91% using Pd-TiO2 while of S. aureus was improved to 94% with Fe-TiO2, showing in this case no significant difference when compared to Ag-TiO2 and Pd-TiO2. In contrast, inactivation of E. coli was not significantly increased when metal modified TiO2 was used, ranging from 47% to 57%. © 2012 Elsevier B.V.

Fe K-edge X-ray absorption spectroscopy study of Pb(Fe2/3W 1/3)O3-PbTiO3 multiferroic ceramics

The present paper is a comprehensive study concerning Fe K-edge X-ray absorption spectroscopy (XAS) measurements, which were performed to characterize the local structure of (1 - x)Pb(Fe2/3W1/3)O 3-xPbTiO3 samples as a function of temperature and PbTiO3 content. Results obtained by the fits of extended X-ray absorption fine structure consist with rhombohedral symmetry for Pb(Fe 2/3W1/3)O3 composition at temperatures lower than room temperature. This result is in apparent disagreement with X-ray and neutron diffraction characterization which have been reported. This apparent disagreement is related to the fact that XAS probes the short-range order, whereas X-ray diffraction provides structural information about the average structure. Moreover, as the PbTiO3 content increases, a disorder has been detected at local structure of the FeO6 octahedron. Analysis of X-ray absorption near edge structure spectra did not show modifications in intensity nor energy of transitions. © 2013 American Institute of Physics.

Concentrations of Cu, Fe, Mn, and Zn in tropical soils amended with sewage sludge and composted sewage sludge

Sewage sludge may be used as an agricultural fertilizer, but the practice has been criticized because sludge may contain trace elements and pathogens. The aim of this study was to compare the effectiveness of total and pseudototal extractants of Cu, Fe, Mn, and Zn, and to compare the results with the bioavailable concentrations of these elements to maize and sugarcane in a soil that was amended with sewage sludge for 13 consecutive years and in a separate soil that was amended a single time with sewage sludge and composted sewage sludge. The 13-year amendment experiment involved 3 rates of sludge (5, 10, and 20 t ha-1). The one-time amendment experiment involved treatments reflecting 50, 100, and 200 % of values stipulated by current legislation. The metal concentrations extracted by aqua regia (AR) were more similar to those obtained by Environmental Protection Agency (EPA) 3052 than to those obtained by EPA3051, and the strongest correlation was observed between pseudo(total) concentrations extracted by AR and EPA3052 and bioavailable concentrations obtained by Mehlich III. An effect of sewage sludge amendment on the concentrations of heavy metals was only observed in samples from the 13-year experiment. © 2012 Springer Science+Business Media B.V.

A new hybrid polyhedral cubic silsesquioxane chemically modified with 4-amino-5-(4-pyridyl)-4H-1,2,4-triazole-3-thiol (APTT) and copper hexacyanoferrate(III) for voltammetric determination of nitrite

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Testing extractants for Cu, Fe, Mn, and Zn in tropical soils treated with sewage sludge for 13 consecutive years

In this paper, we report on a field experiment being carried out in a Typic Eutrorthox. The experiment was initiated in the 1997-98 agricultural season as a randomized block design with four treatments (0, 5, 10, and 20 t ha -1) of sewage sludge and five replicates. Compound soil samples were obtained from 20 subsamples collected at depths of 0-0.1 and 0.1-0.2 m. Cu, Fe, Mn, and Zn concentrations were extracted with DTPA pH 7.3; 0.1 mol L -1 HCl, Mehlich-I, Mehlich-III, and 0.01 mol L-1 CaCl 2. Metal concentrations were determined via atomic absorption spectrometry. Diagnostic leaves and the whole above-ground portion of plants were collected to determine Cu, Fe, Mn, and Zn concentrations extracted by nitric-perchloric digestion and later determined via atomic absorption spectrometry. Sewage sludge application caused increases in the concentrations of soil Cu, Fe, and Mn in samples taken from the 0-0.1 m depth evaluated by the extractants Mehlich-I, Mehlich-III, 0.01 mol L-1 HCl and DTPA pH 7.3. None of the extractants provided efficient estimates of changes in Mn concentrations. The acid extractants extracted more Cu, Fe, Mn, and Zn than the saline and chelating solutions. The highest concentrations of Cu, Fe, and Zn were obtained with Mehlich-III, while the highest concentrations of Mn were obtained with HCl. We did not observe a correlation between the extractants and the concentrations of elements in the diagnostic leaves nor in the tissues of the whole maize plant (Zea mays L.). © 2013 Springer Science+Business Media Dordrecht.

Role of Ca, Fe, Cu and Zn in breast cancer: Study by X-ray fluorescence techniques and immunohistochemical analysis

In recent years, several studies have shown that concentrations of trace elements are altered in neoplastic breast tissues. However, the microenvironment and metabolic changes caused by tumors are complex and still not completely understood. Under this aspect, the combination of different techniques to investigate the role of trace elements in promoting and/or maintaining a tumor is interesting once the combination of information obtained by analytical techniques and immunohistochemical assays, associated with clinicopathological data, may allow a better metabolic understanding of trace elements in breast cancer. In this work, the role of the trace elements Ca, Fe, Cu and Zn in neoplastic breast tissues was investigated by X-ray fluorescence (XRF) techniques and immunohistochemical assays. We determined concentrations of Ca, Fe, Cu and Zn in normal and neoplastic breast tissues using energy dispersive XRF, and these values were used to set the positive or negative expression of elements in normal and neoplastic tissues. These expressions were correlated with the spatial distributions of trace elements (evaluated by micro-XRF) and with immunoexpression of matrix metalloproteinases (MMPs), tissue inhibitors of MMPs and vascular endothelial growth factor. The results revealed that the expression of the trace elements Fe, Cu and vascular endothelial growth factor are related, indicating that higher levels of these elements can be associated with the angiogenic process in breast cancer. Also, associations between Ca, Zn and MMPs expression have been observed, possibly because of the fact that both metals are present in these proteins. © 2013 John Wiley & Sons, Ltd.