Development and validation of a new LC–MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers. Application to some food and feed commodities

A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous determination of six major ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers in food and feed samples. The method involves extraction under alkaline conditions and subsequent clean-up by applying a simple and rapid liquid–liquid partitioning procedure prior to LC–MS/MS analysis. Evaluation of the method revealed good linearity, accuracy and precision. The limits of quantification varied from 0.1 to 1 μg/kg depending on the analyte and matrix. The average extraction and clean-up recoveries in different matrices were between 45 (only for ergometrine in biscuit) and 90%. The uncertainty associated with the analytical method was not higher than 51% and 30%, at concentration levels of 2.5 and 150 μg/kg respectively. Analyte epimerization proved to be minimal during the analytical procedure. The method has been successfully applied to the determination of ergot alkaloids in some Belgian food and feed commodities. Ergot alkaloids were found in 104 out of 122 samples investigated. Ergosine was the most frequently occurring alkaloid, while the highest levels were observed for ergotamine, ergocristine or ergosine, depending on the product type. The total alkaloid content in positive samples varied from 1 to 1145 μg/kg.     

Model selection and optimal sampling in high-throughput experimentation

The practical difficulties encountered in analyzing the kinetics of new reactions are considered from the viewpoint of the capabilities of state-of-the-art high-throughput systems. There are three problems. The first problem is that of model selection, i.e., choosing the correct reaction rate law. The second problem is how to obtain good estimates of the reaction parameters using only a small number of samples once a kinetic model is selected. The third problem is how to perform both functions using just one small set of measurements. To solve the first problem, we present an optimal sampling protocol to choose the correct kinetic model for a given reaction, based on T-optimal design. This protocol is then tested for the case of second-order and pseudo-first-order reactions using both experiments and computer simulations. To solve the second problem, we derive the information function for second-order reactions and use this function to find the optimal sampling points for estimating the kinetic constants. The third problem is further complicated by the fact that the optimal measurement times for determining the correct kinetic model differ from those needed to obtain good estimates of the kinetic constants. To solve this problem, we propose a Pareto optimal approach that can be tuned to give the set of best possible solutions for the two criteria. One important advantage of this approach is that it enables the integration of a priori knowledge into the workflow.     

Patterning of Epitaxial Perovskites from Micro and Nano Molded Stencil Masks

A process is developed that combines soft lithographic molding with pulsed laser deposition (PLD) to make heteroepitaxial patterns of functional perovskite oxide materials. Micro‐ and nanostructures of sacrificial ZnO are made by micro molding in capillaries (MiMiC) and nano transfer molding, respectively, and used to screen the single crystalline substrates during subsequent PLD. ZnO is used because of its compatibility with the high temperatures reached during PLD and because of the ease of its removal after use by benefiting from its amphoteric nature. Sub‐micrometer sized lines of La_0.67Sr_0.33MnO₃ are made by the transfer molding approach, preserving the anisotropic features expected for a fully oriented thin film and taking account for the magnetostatic contribution from the line shapes. Different patterns of SrRuO₃ are made with lateral dimensions of a few micrometers having individual features for which electrical isolation is illustrated. The bottom‐up soft lithographic methods can be compliantly utilized for making epitaxial structures of various shapes and sizes in the μm down to the nm range, and offer unique opportunities for fundamental studies as well as for realizing technological applications.     

Formulation and characterization of anisotropic conductive adhesive paste for microelectronics packaging applications

There has been a steadily increasing interest in using electrically conductive adhesives as interconnecting materials in electronics manufacturing. In this paper, several anisotropic conductive adhesive (ACA) pastes were formulated, which consist of diglycidyl ether of bisphenol F or diglycidyl ether of bisphenol A as polymer matrix, imidazoles as curing agents, and different sizes of silver (Ag) powders or gold (Au)-coated polymer spheres as conductive particles. The effects of ACA resin and different curing agents, as well as different conductive particles, on flexible substrate of the flip-chip joint were studied. The results show that the size and type of different conductive particles have very limited influence on an ACA flip-chip joint. The ACA resin as well as the curing agent can affect the reliability of the joint. The same results can be applied for the failure analysis of ACA flip-chip technology.     

Long‐Range Domain Structure and Symmetry Engineering by Interfacial Oxygen Octahedral Coupling at Heterostructure Interface

In epitaxial thin film systems, the crystal structure and its symmetry deviate from the bulk counterpart due to various mechanisms such as epitaxial strain and interfacial structural coupling, which is accompanyed by a change in their properties. In perovskite materials, the crystal symmetry can be described by rotations of sixfold coordinated transition metal oxygen octahedra, which are found to be altered at interfaces. Here, it is unraveled how the local oxygen octahedral coupling at perovskite heterostructural interfaces strongly influences the domain structure and symmetry of the epitaxial films resulting in design rules to induce various structures in thin films using carefully selected combinations of substrate/buffer/film. Very interestingly it is discovered that these combinations lead to structure changes throughout the full thickness of the film. The results provide a deep insight into understanding the origin of induced structures in a perovskite heterostructure and an intelligent route to achieve unique functional properties.     

WCDMA的分层式体系结构

分层式体系结构简介 WCDMA的分层式体系结构主要负责媒体网关(MGW)的分配和移动交换中心(MSC)服务器的集中管理.它具有分布式交换功能,并集中进行运营维护和呼叫控制,可大大降低运营开销.     

Microwave-transmission, heat and temperature properties of electrically conductive adhesive

Microwave heating significantly speeds up the curing process of polymer and polymer-based composites. The present theoretical work studies the microwave transmission through the electrically conductive adhesive (ECA), heat generation and transfer inside the ECA and subsequently the microwave heating rate of the ECA. By studying the temporal transmission property of the microwaves in the ECA, we have calculated quantitatively the electromagnetic field distribution around a metal filler. It has been shown that the penetration depth of the skin effect in the metal filler is significantly smaller than the one of a bulk metal material. The heat generation (microwave power absorption) is negligible in the metal filler due to its large electric conductivity. Furthermore, due to the high thermal conductivity, the thermal equilibrium between the metal filler and the surrounding adhesive is reached within a nano second (10/sup -9/ s). The temperature of the whole ECA system becomes uniform within a time interval of 10/sup -3/ s. When the temperature of the system is relatively low, the heating rate of the system is linearly proportional to the external microwave input power and the heating time. It gradually saturates when the temperature of the ECA is so high that the heat radiation from the ECA becomes significant. Numerical results of our theoretical model agree well with experimental data, thus providing a solid platform for designing the microwave curing process of the ECA.     

The link between ethnic diversity and scientific impact: the mediating effect of novelty and audience diversity

Scientometrics - Understanding the nature and value of scientific collaboration is essential for sound management and proactive research policies. One component of collaboration is the composition...     

Seed-mediated grown platinum nanocrystal: A correlation between seed volume and catalytic performance of formic acid and ethanol oxidation

Platinum (Pt) nanocrystals of cubic and octopod structures were synthesized via seed-mediated solvothermal growth with monoethanolamine as the solvent. The combination of nanocube and octopod structures was formed using 0.025 ml seeds loading, while increasing the seeds volume to 0.050 ml and 0.100 ml produced nanocube as the primary product. The octopod structure evolves from the overgrown nanocube via kinetic growth mechanism. Pt nanocube formed with 0.050 ml seeded solution has the potential to serve as a catalyst in formic acid oxidation by virtue of its high electrochemical surface area of 10.93 m²/g, over that of Pt black at 8.62 m²/g and resistance to poisonous CO. Nonetheless, it is less catalytically active in ethanol oxidation as depicted by the small electrochemical surface area of 8.64 m²/g and low current density in longer period.