Analysis of ochratoxin A in milk after direct immunoaffinity column clean-up by high-performance liquid chromatography with fluorescence detection

The present work describes a new analytical method for direct immunoaffinity column clean-up of ochratoxin A (OTA) in milk samples followed by determination of the toxin using high-performance liquid chromatography with fluorescence detection (HPLC-FD). Two different immunoaffinity cartridges (IAC) were investigated, and Ochraprep columns were chosen because they showed the best results. An average recovery of 89.8% and a mean RSD of 5.8% for artificially contaminated cow's milk in the range of 5-100 ng/L were attained. The calculated limit of detection (LOD) and limit of quantitation (LOQ) were as low as 0.5 and 5 ng/L, respectively. This new easy and fast method avoids a previous liquid-liquid extraction step and therefore the use of toxic chlorinated solvents. Chromatograms of the final extracts were clean and OTA could be easily detected at a retention time of 8.4 min without interferences. To assess the presence of the toxin in cow's milk eight samples of skimmed and four samples of whole milk were analysed and OTA was not detected over the established detection limit.     

Synthesis and acid digestion of biomorphic ceramics: determination of alkaline and alkaline earth ions

Ceramic and glass are some of the more recent engineering materials and those that are most resistant to environmental conditions. They belong to advanced materials in that they are being developed for the aerospace and electronics industries. In the last decade, a new class of ceramic materials has been the focus of particular attention. The materials were produced with natural, renewable resources (wood or wood-based products). In this work, we have synthesised a new biomorphic ceramic material from oak wood and Si infiltration. After the material characterization, we have optimized the dissolution of the sample by acid attack in an oven under microwave irradiation. Experimental designs were used as a multivariate strategy for the evaluation of the effects of varying several variables at the same time. The optimization was performed in two steps using factorial design for preliminary evaluation and a Draper-Lin design for determination of the critical experimental conditions. Five variables (time, power, volume of HNO3, volume H2SO4 and volume of HF) were considered as factors and as a response the concentration of different metal ions in the optimization process. Interactions between analytical factors and their optimal levels were investigated using a Draper-Lin design.     

High-temperature thermal behaviour of Cr-Doped LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> spinels synthesized by the sucrose-aided combustion method

Chromium doped spinels LiCr_YMn_2−YO₄ (0.2≤Y≤0.8) has been synthesized by the sucrose-aided combustion procedure. The thermal behaviour, phase homogeneity and structural characteristics of the samples were studied by thermal analysis, coupled mass spectrometry, and room-and high-temperature X-ray diffraction methods. It was found that the ‘as prepared’ samples contained residual organic impurities undetectable for X-ray diffraction, that burn out completely at 400°C. Samples treated between 400 and 750°C are single phase spinels, whose crystallites size increase from 10 to 50 nm on increasing the temperature. Cr-doping enhances the thermal stability of the spinels, which augments on increasing the Cr content Y. The enhanced thermal stability of the spinels has been accounted for based on the high excess stabilization energy of Cr³⁺ in octahedral ligand field.     

Retention of lysozyme activity by physical immobilization in nanocellulose aerogels and antibacterial effects

Aerogels prepared from aqueous dispersions of anionic and cationic cellulose nanofibrils (CNFs) were investigated as solid supports for enzymes and silver nanoparticles and to elicit a sustained antibacterial effect. The imparted stabilization in dry conditions was studied with aerogels that were cast after mixing the enzymes with CNFs followed by dehydration (freeze-drying). The activity of lysozyme immobilized in the given CNF system was analyzed upon storage in liquid and air media. In contrast with aqueous solutions of free, unbound enzyme, which lost activity after the first day, the enzyme immobilized physically in unmodified and cationic CNF presented better stability (activity for a longer time). However, the enzyme activity was reduced in the case of anionic CNF, which was prepared by TEMPO-mediated oxidation (TO-CNF). Both humidity and temperature reduced the stability of the enzyme immobilized in the respective CNF aerogel. The antibacterial activity of CNF aerogels carrying lysozyme was also tested against gram-negative and gram-positive bacteria. The results were compared with those obtained from CNF systems loaded with silver nanoparticles (AgNP) after in situ synthesis via UV reduction. Storage in cold or dry conditions preserved the activity and antibacterial performance of enzyme-loaded CNF aerogels. As expected, the lysozyme-containing aerogels showed lower inhibition than the AgNP-containing aerogel. In this latter case, the antibacterial activity depended on the concentration and size of the nanoparticles. Compared to unmodified CNF and TO-CNF, the aerogels prepared with cationic CNF, loaded with either lysozyme or AgNPs, showed remarkably better antibacterial activity. Similar experiments were conducted with horseradish peroxidase, which confirmed, to different degrees, the observations derived from the lysozyme systems. Overall, the results indicate that non-toxic and biodegradable CNF is a suitable support for bio-active materials and is effective in protecting and retaining enzymatic and antibacterial activities.     

Kinetic-fluorimetric determination of microamounts of cerium(IV) by means of sodium 4,8-diamino-1,5-dihydroxyanthraquinone-2,6-disulphonate

Summary A kinetic method for determination of traces of Ce(IV), based on the oxidation of sodium 4,8-diamino-1,5-dihydroxyanthraquinone-2, 6-disulphonate is described. The reaction is monitored by means of the fluorescence of the oxidation product ( _ex=525nm, _em=585 nm), and allows determination of 0.02–0.37 ppm Ce(IV). The proposed method has few interferences.

---

Kinetisch-fluorimetrische Bestimmung von Mikromengen Cer(IV) mit Natnum-4,8-diamino-1,5-dihydroxyanthrachinon-2,6-disulfonat

Zusammenfassung Eine kinetische Methode zur Bestimmung von Spuren Cer(IV) mit Hilfe von Natrium-4,8-diamino-1,5-dihydroxyanthrachinon-2,6-disulfonat wurde beschrieben. Dabei wird ein fluoreszierendes Oxydationsprodukt gebildet, das bei 525 nm angeregt mit einer maximalen Emission bei 585 nm fluoresziert. Die Reaktion ermöglicht die Bestimmung von 0,02–0,37 ppm Cer(IV). Die vorgeschlagene Methode wird nur durch wenige Störungen eingeschränkt.

     

Products of Jacobians as Prym-Tyurin varieties

Let X ₁, ..., X _m denote smooth projective curves of genus g _i ≥ 2 over an algebraically closed field of characteristic 0 and let n denote any integer at least equal to . We show that the product JX ₁ × ... × JX _m of the corresponding Jacobian varieties admits the structure of a Prym-Tyurin variety of exponent n ^m-1. This exponent is considerably smaller than the exponent of the structure of a Prym-Tyurin variety known to exist for an arbitrary principally polarized abelian variety. Moreover it is given by explicit correspondences.      

Transmission of macroeconomic shocks to risk parameters: Their uses in stress testing

In this paper, we are interested in evaluating the resilience of financial portfolios under extreme economic conditions. Therefore, we use empirical measures to characterize the transmission process of macroeconomic shocks to risk parameters. We propose the use of an extensive family of models, called General Transfer Function Models, which condense well the characteristics of the transmission described by the impact measures. The procedure for estimating the parameters of these models is described employing the Bayesian approach and using the prior information provided by the impact measures. In addition, we illustrate the use of the estimated models from the credit risk data of a portfolio.     

Selecting an Effective Entropy Estimator for Short Sequences of Bits and Bytes with Maximum Entropy

Entropy makes it possible to measure the uncertainty about an information source from the distribution of its output symbols. It is known that the maximum Shannon’s entropy of a discrete source of information is reached when its symbols follow a Uniform distribution. In cryptography, these sources have great applications since they allow for the highest security standards to be reached. In this work, the most effective estimator is selected to estimate entropy in short samples of bytes and bits with maximum entropy. For this, 18 estimators were compared. Results concerning the comparisons published in the literature between these estimators are discussed. The most suitable estimator is determined experimentally, based on its bias, the mean square error short samples of bytes and bits.     

Supershell structure in alkali metal nanowires

Nanowires are formed by indenting and subsequently retracting two pieces of sodium metal. Their cross section gradually reduces upon retraction and the diameters can be obtained from the conductance. In previous work we have demonstrated that when one constructs a histogram of diameters from large numbers of indentation-retraction cycles such histograms show a periodic pattern of stable nanowire diameters due to shell structure in the conductance modes. Here, we report the observation of a modulation of this periodic pattern, in agreement with predictions of a supershell structure.