Preliminary ionome of the parotoid gland secretion from Rhinella jimi toad.

The cururu toad (Rhinella jimi) is an anuran belonging to the fauna of the Brazilian northeast region, which releases a secretion with toxins from your parotoid glands. Although it has some information about secondary metabolites and proteins, the elemental composition of the released secretion is unknown. Therefore, this is the first report on the ionome of the secretion of the parotoid glands from R. jimi, investigating the influences of abiotic factors such as biome, seasonality, and gender. ICP-MS was used for measurements combined with principal component analysis (PCA). A screening of the secretion sample detected 68 elements which the total concentration of 18 elements was determined. PCA revealed that biome and seasonality factors have a greater influence on the ionomic profile of parotoid secretion. The presence of toxic metals in the secretion samples indicates that the R. jimi toad can be considered a potential bioindicator. These findings may contribute to understanding the metabolism, lifestyle, and interaction of the R. jimi toad with environmental factors as well as open new perspectives to investigate the relationships of the ionome with other biomolecules, for example, metalloproteins and their physiological functions.

In vitro gastrointestinal digestion to evaluate the total, bioaccessible and bioavailable concentrations of iron and manganese in açaí (Euterpe oleracea Mart.) pulps.

Açaí pulp consumption has increased in Brazil and worldwide. Recently, a high average content of manganese (450 mg/kg) was observed in açaí pulp, raising the hypothesis of toxicological effects associated to its ingestion. However, the total concentration of an element does not reflect the real benefits and risks of consuming a food. In this context, the total, bioaccessible and bioavailable concentrations of Fe and Mn were assessed in 9 açaí pulps. Fe and Mn contents ranged from 27.6 to 73 and from 145 to 1197 mg kg-1, respectively. Fe and Mn bioaccessibilities represented from 29 to 40 and from 39 to 55% of total amounts. Fe bioavailabilities were lower than LOQ and those of Mn varied from 8 to 17% of total. A daily consumption of 100 g of açaí pulp exceeds by at least 1.5-fold the recommended Mn daily intakes for adults whereas poorly contributes to Fe intakes. Since the lowest Mn bioaccessible and bioavailable fraction corresponded to a Mn intake value higher than the tolerable upper intakes for children and that high amounts of Mn intake may impair Fe absorption, higher açaí consumption may be worrisome. Future nutritional, toxicological and speciation studies must be undertaken.

Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively.

Improved antibacterial activity of nanofiltration polysulfone membranes modified with silver nanoparticles.

Polysulfone membranes (PSf) containing silver nanoparticles were prepared by the wet phase-inversion process. Silver nanoparticles (AgNP) were dispersed into the polymer matrix using two different methodologies. In the first one, the AgNP were synthesized and further dispersed into the polymer solution (ex situ process). In the second method, the formation of the AgNP was performed in situ. The AgNP crystalline structure in the PSf membranes was confirmed by X-ray diffraction. Field emission scanning electron microscopy images showed that the addition of AgNP in PSf membranes caused no significant changes to the finger-like morphology. When the ex situ methodology was applied, 45 nm average size AgNP were uniformly distributed in the internal pores of the membranes. However, when the AgNP were formed through the in situ process, the AgNP were uniformly and preferentially distributed on the top and bottom surfaces of the membrane. In the last case, the AgNP showed cubic morphology when present in the bottom and top surfaces, however, when inside the membrane their morphology was spherical. The cubic-like nanoparticles displayed a 38 nm average edge length. The silver ion released from the membrane during water filtration was measured using inductively coupled plasma mass spectrometry, which showed a silver leaching of approximately 2 µg L(-1). The nanocomposite membranes prepared by the in situ method exhibited a better antibacterial activity, in comparison to those prepared by ex situ, and also a decrease in 90% Escherichia coli adhered cells compared to the pristine PSf membranes. In conclusion, the in situ procedure can be considered a feasible, simple, and reproducible methodology to prepare anti-biofouling polysulfone membranes containing AgNP.

Feasibility of internal standardization in the direct and simultaneous determination of As, Cu and Pb in sugar-cane spirits by graphite furnace atomic absorption spectrometry.

Bismuth and Sb were evaluated as internal standards (IS) to minimize matrix effects on the direct and simultaneous determination of As, Cu, and Pb in cachaça by graphite furnace atomic absorption spectrometry using W-coated platform plus Pd-Mg(NO(3))(2) as modifier. For 20microL injected sample, calibration within the 0.5-10microg L(-1) As, 100-1000microg L(-1) Cu and 0.5-30microg L(-1) Pb intervals were established using the ratios As absorbance to Sb absorbance, Cu absorbance to Bi absorbance and Pb absorbance to Bi absorbance versus analytes concentration, respectively. Typical linear correlations of 0.998, 0.999 and 0.999 were, respectively, obtained. The proposed method was applied for direct determination of As, Cu and Pb in 10 commercial cachaça samples and results were in agreement with those obtained by inductively coupled plasma mass spectrometry at 95% confidence level. The found characteristic masses were 30pg As, 274pg Cu and 39pg Pb. The useful lifetime of the graphite tube was around 760 firings. Recoveries of As, Cu and Pb added to cachaça samples varied, respectively, from 98% to 109%, 97% to 108% and 98% to 104% with internal standards and from 48% to 54%, 53% to 92% and 62% to 97% without internal standards. The limits of detection were 0.13microg L(-1) As, 22microg L(-1) Cu and 0.05microg L(-1) Pb. The relative standard deviations (n=12) for a spiked sample containing 20microg L(-1) As, Pb and 500microg L(-1) Cu were 1.6%, 1.0%, and 1.8% with IS and 4.3%, 5.2%, and 5.5% without IS.

Evaluation of alternate lines of Fe for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry.

The usefulness of the secondary line at 252.744nm and the approach of side pixel registration were evaluated for the development of a method for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The influence of side pixel registration on the sensitivity and linearity was investigated by measuring at wings (248.325, 248.323, 248.321, 248.329, and 248.332nm) of the main line for Fe at 248.327nm. For the secondary line at 252.744nm or side pixel registration at 248.325nm, main lines for Cu (324.754nm), Mn (279.482nm) and Zn (213.875nm), sample flow-rate of 5.0mLmin(-1) and calibration by matrix matching, analytical curves in the 0.2-1.0mgL(-1) Cu, 1.0-20.0mgL(-1) Fe, 0.2-2.0mgL(-1) Mn, 0.1-1.0mgL(-1) Zn ranges were obtained with linear correlations better than 0.998. The proposed method was applied to seven soil samples and two soil reference materials (IAC 277; IAC 280). Results were in agreement at a 95% confidence level (paired t-test) with reference values. Recoveries of analytes added to soil extracts containing 0.15 and 0.30mgL(-1) Cu, 7.0 and 14mgL(-1) Fe, 0.60 and 1.20mgL(-1) Mn, 0.07 and 0.15mgL(-1) Zn, varied within the 94-99, 92-98, 93-101, and 93-103% intervals, respectively. The relative standard deviations (n=12) were 2.7% (Cu), 1.4% (Fe - 252.744nm), 5.7% (Fe - 248.325nm), 3.2% (Mn) and 2.8% (Zn) for an extract containing 0.35mgL(-1) Cu, 14mgL(-1) Fe, 1.1mgL(-1) Mn and 0.12mgL(-1) Zn. Detection limits were 5.4microgL(-1) Cu, 55microgL(-1) Fe (252.744nm), 147microgL(-1) Fe (248.325nm), 3.0microgL(-1) Mn and 4.2microgL(-1) Zn.