Evaluation of Cu, Mn, and Se in Vegetables Using Ultrasonic Extraction and GFAAS Quantification

This paper proposes a method for the determination of copper, manganese, and selenium in vegetables of conventional and organic farming in the state of So Paulo/Brazil using ultrasonic extraction of analytes and subsequent quantification by graphite furnace atomic absorption spectrometry (GFAAS). Using 0.10 mol L(-1) of hydrochloric acid as the extracting solution, the following optimal extraction conditions were established: sample mass of 100 mg, sample grain size of < 60 mu m, sonication time of five cycles of 40 s, and sonication power of 136 W. The analytes were determined by GFAAS, applying drying temperatures of 90 A degrees C to 250 A degrees C, pyrolysis temperature of 1,300 A degrees C, atomization temperature of 2,300 A degrees C, and cleaning temperature of 2,800 A degrees C. Palladium nitrate was co-injected with the samples as a chemical modifier and tungsten as a permanent modifier. The accuracy and precision of the proposed extraction method were evaluated based on a certified standard, RM 8433 Corn Bran (NIST RM 8433). The results obtained by the ultrasonic extraction method were equivalent to those obtained by the method of acid mineralization of samples in a microwave oven. However, the proposed methodology reduces the analytical time considerably, favoring the analytical speed. Moreover, the quantity of residues generated and discharged into the environment is also considerably lower.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

GFAAS Determination of Zinc in Fish Feed and Feces Using Slurry Sampling

This paper presents a simple, fast, and sensitive method to determine zinc in samples of feces and fish feed by electrothermal atomic absorption spectrometry through the direct introduction of slurries of the samples into the spectrometer's graphite tube. The procedure is based on the injection of 10 mu L of an acidified aqueous solution containing 0.50% w/v of feces or feed and 0.50% v/v HNO(3) into graphite tube. The limits of detection and quantification calculated for 20 readings of the blank of the standard slurries (0.50% w/v of feces or feed devoid of zinc) were 0.04 and 0.13 mu g L(-1) for the standard feces slurries and 0.05 and 0.17 mu g L(-1) for the standard feed slurries. The proposed method was applied in studies of digestibility of zinc in different fish feeds, and their results proved compatible with that obtained from samples mineralized by acid digestion using microwave oven

Evaluation of pH and calcium ion release of new root-end filling materials

Objective. The purpose of this study was to evaluate the pH and calcium ion release of 6 materials used for root-end filling and perforation repair. Study design. Gray ProRoot MTA, gray MTA-Angelus, white MTA-Angelus, and CPM were compared to 2 experimental ones: MTA-exp, also based in Portland cement with a modified mixing liquid, and MBPc, an epoxy-resin based cement containing calcium hydroxide. After 3, 24, 72, and 168 hours the water in which each sample had been immersed was tested to determine the ph and calcium ion release. Results. All the analyzed materials showed alkaline pH and capacity to release calcium ions; however, a tendency of reduction of these characteristics was noted for all the analyzed materials, except for the MBPc, which showed a slight increase of pH among the 3 initial periods. Conclusion. The results suggest that all materials investigated presented alkaline pH and ability of release of calcium ions. (Oral Surg Oral Med Oral Pathol Oral Radiol Endod 2009; 108: 135-139

Metal ions bound to the human milk immunoglobulin A: Metalloproteomic approach

The presence of calcium, iron, and zinc bound to human milk secretory IgA (sIgA) was investigated. The sIgA components were first separated by two-dimensional polyacrylamide gel electrophoresis and then identified by electrospray ionization-tandem mass spectrometry (ESI MS MS). The metal ions were detected by flame atomic absorption spectrometry after acid mineralization of the spots. The results showed eight protein spots corresponding to the IgA heavy chain constant region. Another spot was identified as the transmembrane secretory component. Calcium was bound to both the transmembrane component and the heavy chain constant region, while zinc was bound to the heavy chain constant region and iron was not bound with the identified proteins. The association of a metal ion with a protein is important for a number of reasons, and therefore, the findings of the present study may lead to a better understanding of the mechanisms of action and of additional roles that sIgA and its components play in human milk. (C) 2014 Elsevier Ltd. All rights reserved.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES

Bioanalytical methods for the metalloproteomics study of bovine longissimus thoracis muscle tissue with different grades of meat tenderness in the Nellore breed (Bos indicus)

The work describes a metalloproteomics study of bovine muscle tissue with different grades of meat tenderness from animals of the Nellore breed (Bos indicus) based on protein separation by two-dimensional gel electrophoresis, the identification of calcium ions in protein spots by X-ray fluorescence (SR-XRF) and the characterisation of proteins by electrospray ionisation mass spectrometry. Forty (40) specimens were selected and divided into two experimental groups: animals with tough meat (TO) and animals with tender meat (TE). A third group (P) of Piedmontese breed animals (Bos taurus) was included to serve as a comparative model for the level of meat tenderness. The procedures were efficient and preserved the metal protein structure, enabling calcium detection in protein spots by SR-XRF at a given molecular weight range of 14-97 kDa. Two proteins (pyruvate kinase and albumin) were inferred to be related to the phenotypical differences in animals from the different groups. (C) 2014 Elsevier Ltd. All rights reserved.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES

Metallomic study on plasma samples from Nile tilapia using SR-XRF and GFAAS after separation by 2D PAGE: initial results

An investigation was made on plasma samples obtained after protein separation. The proteome of the plasma of Nile tilapia (Oreochromis niloticus) was separated by 2D PAGE, and manganese and zinc in protein spots was qualitatively and quantitatively determined by synchrotron radiation X-ray fluorescence (SR-XRF) and graphite furnace atomic absorption spectrometry (GFAAS). Manganese and zinc are present in four and six plasma protein spots, respectively. These ions are bound to proteins with molecular weights ranging from 19 to 70 kDa and with isoelectric point (pI) ranging from 4.7 to 6.3. The concentrations of manganese and zinc bound to these proteins as determined by GFAAS following acid digestion of the spots range from 0.8 to 2.6 mg of manganese, and from 1.0 to 6.3 mg of zinc, respectively, per g of protein.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq