Assessment of total concentration and bioaccessible fraction of minerals in peaches from different cultivars by MIP OES.

This paper describes studies for the determination of total concentration and bioaccessible fraction of minerals in peaches by MIP OES. The PCA analysis identified 3 distinct groups of elements concerning the total concentration, which was attributed to the origin of each cultivar. Among the macroelements, K presented higher values for total concentration, while B and Fe predominated among the microelements. Regarding the bioaccessible fraction, Mn presented the highest percentage (46-84%), followed by Zn and B (10-63% and 33-57%, respectively). Pearson's correlation coefficient revealed that reducing sugars and titratable acidity can influence the mineral bioaccessibility, highlighting the strong positive correlations between reducing sugars with Mn and total acidity with Fe. Peach cultivars have satisfactory nutritional value, but the total and bioaccessible concentrations of minerals obtained do not meet the recommended daily needs, requiring the consumption of other fruits and vegetables to complement the diet.

Evaluation of the use of a reflux system for sample preparation of processed fruit juices and subsequent determination of Cr, Cu, K, Mg, Na, Pb and Zn by atomic spectrometry techniques.

The acid decomposition method was applied for the sample preparation of processed fruit juice. The decomposition of 15mL of juice sample using HNO3 and H2O2 was performed in a digester block with reflux system and heated at 200°C for 150min. The limits of detection were 0.03; 0.24; 0.8; 0.008; 0.026 and 0.056mgL-1 for Cr, Cu, K, Mg, Na and Zn, respectively and for Pb was 0.99µgL-1. The accuracy was evaluated by spiked experiments (80 to 119%). Four processed fruit juice samples commercialized in Brazil (strawberry, mango, peach, and orange) were analyzed and indicated the absence of Cr, Zn and Cu in the samples, except for Cu in strawberry juice. Pb was found in the mango juice sample (17.8±0.9µgL-1) and the concentration is below the maximum values recommended by Brazilian legislation for juices of citric fruits (0.3mgkg-1).

Evaluation of pH and calcium ion release of a dual-cure bisphenol A ethoxylate dimethacrylate/mineral trioxide aggregate-based root-end filling material.

INTRODUCTION: The incorporation of light-curable resins has been proposed for mineral trioxide aggregate (MTA) to improve its properties and reduce its setting time. The aim of the present study was to assess the pH and calcium ion release of an experimental bisphenol A ethoxylate dimethacrylate/MTA-based root-end filling material (E-MTA) in comparison with white MTA Angelus (Angelus, Londrina, PR, Brazil) (W-MTA) and to evaluate the influence of the addition of calcium chloride (CaCl2) on these properties. METHODS: Polyethylene tubes filled with the materials were immersed in deionized water for the measurement of pH (digital pH meter) and calcium release (atomic absorption spectrophotometry). The evaluations were performed at 3 and 24 hours and 7, 15, and 30 days. Data were measured using 2-way repeated measures of variance followed by the Holm-Sidak method (P < .05). RESULTS: All materials presented a reduction in the pH and released calcium ions during the 30 days of the study. E-MTA showed a significantly lower calcium ion release capacity when compared with W-MTA (P < .05). The calcium release of E-MTA + 5% CaCl2 was similar to W-MTA (P > .05). CONCLUSIONS: The monomer bisphenol A ethoxylate dimethacrylate added to MTA formed a material with a lower capacity of calcium release than W-MTA despite maintaining a similar pH. However, the addition of CaCl2 improved the calcium release of this material.

Determination of platinum originated from antitumoral drugs in human urine by atomic absorption spectrometric methods.

Cisplatin and carboplatin are the most common platinum-based drugs used in cancer treatment. Pharmacokinetic investigations, the evaluation of the body burden during the treatment, as well as baseline levels of platinum in humans have attracted great interest. Thus, accurate analytical methods for fast and easy Pt monitoring in clinical samples become necessary. In the present study atomic absorption spectrometric methods for the determination of platinum in the forms of cisplatin and carboplatin in human urine were investigated. Platinum, in these different forms, could be determined in urine, after simple sample dilution. Regarding electrothermal atomic absorption spectrometry, the optimum parameters were defined by a central composite design optimization. Multiplicative matrix effects were overcome by using a mixture of HCl and NaCl as modifier. The limit of detection (LOD) was 0.004 mgL(-1) of platinum in the original sample. For the analysis of more concentrated samples, high resolution continuous source flame atomic absorption spectrometry was also investigated. Flame conditions were optimized by a multivariate D-optimal design, using as response the sum of the analyte addition calibration slopes and their standard deviations. Matrix matched external calibration with PtCl(2) calibration solutions, was possible, and the LOD was 0.06 mgL(-1) in the original sample. The results obtained by the proposed procedures were also in good agreement with those obtained by an independent comparative procedure.

Simultaneous on-line pre-concentration and determination of trace metals in environmental samples by flow injection combined with inductively coupled plasma mass spectrometry using silica gel modified with niobium(V) oxide.

This work presents the development of an on-line pre-concentration system for simultaneous determination of Cd, Cu, Ni, V, Zn, Co and Pb in aqueous environmental samples and detection by inductively coupled plasma mass spectrometry. The system is based on cationic retention of the analytes onto a mini-column filled with silica gel modified with niobium(V) oxide. The effects of chemicals and flow variables have been investigated. The optimized operating conditions, selected as a compromise between sensitivity and analytical frequency were: sample pH 7.0, sample flow rate of 6.0mL min(-1), eluent flow rate of 2.0mL min(-1), and eluent (HNO(3)) concentration of 2.5mol L(-1). The relative standard deviation (n=7), enrichment factor and linear working range were 0.8-4.5%, 23.3-37.2 and 0.05-25.0microg L(-1), respectively. Limits of detection were between 0.01 and 0.03microg L(-1). The accuracy of the proposed method was checked with certified materials (NASS-4, NASS-5, CASS-4 and SRM 1643e). Values obtained were in accordance with those reported for the certified materials. Recovery was found to be in the range of 90-110% for a suit of water samples with variable matrices (seawater, tap water and ground water) collected in Florianopolis, Brazil.

Slurry sampling of sediments and coals for the determination of Sn by HG-GF AAS with retention in the graphite tube treated with Th or W as permanent modifiers.

A method for the determination of Sn in slurry samples of sediment and coal by hydride generation graphite furnace electrothermal atomic absorption spectrometry (HG-GF AAS) is proposed. The slurries were prepared by mixing the ground sample (particle size < or =50 microm) with 2.0 mol L(-1) HCl for the sediment samples or with 2.0 mol L(-1) HCl+1.0% v/v HF in a saturated boric acid medium for the coal samples. The slurry was placed in an ultrasonic bath for 30 min, before and after standing for 24 h, with occasional manual stirring. The graphite tube was treated with 0.5 mg of Th or W as a permanent modifier. Sn determination was carried out by electrothermal atomic absorption spectrometry at the optimized retention temperatures of 450 and 300 degrees C for Th and W treatment, respectively. With this coupling, kinetic interference in the formation of the hydrides is avoided, and excellent detection limits can be obtained by using peak height. For the chemical vapor generation device, an optimized volume of 2 mL of sample slurry and an optimized NaBH4 concentration of 5% m/v were employed. The vapor produced was transported and retained on the graphite tube surface, which was further heated for Sn atomization. The accuracy of the method was verified by analyzing five certified sediments and three coals. By using the external calibration against aqueous standard solutions, the results obtained were in agreement with the certified values only for the sediment samples. For the coal samples, an addition calibration curve, obtained for one certified coal, was necessary to achieve accurate results. The obtained limits of detection were 0.03 microg g(-1) for sediment and 0.09 microg g(-1) for coal with Th as permanent modifier. The relative standard deviations were lower than 15%, demonstrating an adequate precision for slurry analysis. Sediment and coal samples from Santa Catarina, Brazil, were also analyzed.