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A novel, cost-efficient method for the analytical extraction of the Fusarium mycotoxin zearalenone (ZON) from edible oils by dynamic covalent hydrazine chemistry (DCHC) was developed and validated for its application with high performance liquid chromatography-fluorescence detection (HPLC-FLD). ZON is extracted from the edible oil by hydrazone formation on a polymer resin functionalised with hydrazine groups and subsequently released by hydrolysis. Specifity and precision of this approach are superior to liquid partitioning or gel permeation chromatography (GPC). DCHC also extracts zearalanone (ZAN) but not α-/β-zearalenol or -zearalanol. The hydrodynamic properties of ZON, which were estimated using molecular simulation data, indicate that the compound is unaffected by nanofiltration through the resin pores and thus selectively extracted. The method's levels of detection and quantification are 10 and 30 μg/kg, using 0.2 g of sample. Linearity is given in the range of 10–20,000 μg/kg, the average recovery being 89%. Bias and relative standard deviations do not exceed 7%. In a sample survey of 44 commercial edible oils based on various agricultural commodities (maize, olives, nuts, seeds, etc.) ZON was detected in four maize oil samples, the average content in the positive samples being 99 μg/kg. The HPLC-FLD results were confirmed by HPLC–tandem mass spectrometry and compared to those obtained by a liquid partitioning based sample preparation procedure.  相似文献   
33.
Silver nanolayers sputtered on polytetrafluoroethylene and their changes induced by post‐deposition annealing at 100–300 °C are studied. Changes in surface morphology and roughness are examined by atomic force microscopy and by measurement of electrical sheet resistance by two‐point technique. Chemical composition was determined by X‐ray photoelectron spectroscopy (XPS) and electrokinetic analysis in dependence on the gold layer thickness. The annealing at 300 °C leads to significant rearrangement of the silver layer, and the transition threshold increases to 35 nm. The presence of oxidized structures on silver‐coated samples is observed in XPS spectra and by electrokinetic analysis, too. Annealing of pristine and silver‐coated poly(tetrafluoroethylene) at 300 °C results in significant change of the sample surface morphology and chemistry. There is observed formation of isolated silver islands on the surface, which could be connected with silver melting. Later, the silver agglomeration takes place. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   
34.
Proteomic analysis of simulated occupational jet fuel exposure in the lung   总被引:3,自引:0,他引:3  
We analyzed protein expression in the cytosolic fraction prepared from whole lung tissue in male Swiss-Webster mice exposed 1 h/day for seven days to aerosolized JP-8 jet fuel at concentrations of 1000 and 2500 mg/m3, simulating military occupational exposure. Lung cytosol samples were solubilized and separated via large scale, high resolution two-dimensional electrophoresis (2-DE) and gel patterns scanned, digitized and processed for statistical analysis. Significant quantitative and qualitative changes in tissue cytosol proteins resulted from jet fuel exposure. Several of the altered proteins were identified by peptide mass fingerprinting, confirmed by sequence tag analysis, and related to impaired protein synthetic machinery, toxic/metabolic stress and detoxification systems, ultrastructural damage, and functional responses to CO2 handling, acid-base homeostasis and fluid secretion. These results demonstrate a significant but comparatively moderate JP-8 effect on protein expression and corroborate previous morphological and biochemical evidence. Further molecular marker development and mechanistic inferences from these observations await proteomic analysis of whole tissue homogenates and other cell compartment, i.e., mitochondria, microsomes, and nuclei of lung and other targets.  相似文献   
35.
The synthesis of 3-amino-7-chloro-1-ethyl-6-fluoro-4(1H)quinolinone derivatives is described. These were investigated for their antibacterial activity.  相似文献   
36.
A general strategy for the synthesis of oligobipyridine ligands 2 – 5 containing from two to five 2,2′-bipyridine subunits, for helical metal complexes is described (sec Scheme). Both the unsubstituted parent strands ( a series) as well as their derivatives bearing fester or amide functions in the 4,4′-positions of the bipyridine moieties ( b – d series) have been obtained.  相似文献   
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We prove that a substitutive dynamical system of Pisot type contains a factor which is isomorphic to a minimal rotation on a torus. If the substitution is unimodular and satisfies a certain combinatorial condition, we prove that the dynamical system is measurably conjugate to an exchange of domains in a self-similar compact subset of the Euclidean space.

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39.
The Toolkit for Accurate Scientific Software (TASS) is a suite of integrated tools for the formal verification of programs used in computational science, including numerically-intensive message-passing-based parallel programs. While TASS can verify a number of standard safety properties (such as absence of deadlocks and out-of-bound array indexing), its most powerful feature is the ability to establish that two programs are functionally equivalent. These properties are verified by performing an explicit state enumeration of a model of the program(s). In this model, symbolic expressions are used to represent the inputs and the values of variables. TASS uses novel techniques to simplify the symbolic representation of the state and to reduce the number of states explored and saved. The TASS front-end supports a large subset of C, including (multi-dimensional) arrays, structs, dynamically allocated data, pointers and pointer arithmetic, functions and recursion, and other commonly used language constructs. A number of experiments on small but realistic numerical programs show that TASS can scale to reasonably large configurations and process counts. TASS is open source software distributed under the GNU Public License. The Java source code, examples, experimental results, and reference materials are all available at .  相似文献   
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