Simultaneous determination of cucurbitacin IIa and cucurbitacin IIb of Hemsleya amabilis by HPLC–MS/MS and their pharmacokinetic study in normal and indomethacin‐induced rats

A selective and sensitive HPLC–MS/MS method was developed for the simultaneous determination of cucurbitacin IIa (cuIIa) and cucurbitacin IIb (cuIIb), the major bioactive cucurbitacins of Hemsleya amabilis, in rat plasma using euphadienol as internal standard (IS). After liquid–liquid extraction with dichloromethane, separation was achieved on a Syncronis HPLC C₁₈ column (150 mm × 4.6 mm, 5 μm) using an isocratic mobile phase system consisting of acetonitrile–water (85:15, v/v) at a flow rate of 0.6 mL/min with a split ratio of 1:2. Detection was performed on a TSQ Quantum Ultra mass spectrometer equipped with an positive‐ion electrospray ionization source. The lower limits of quantification (LLOQs) were 0.25 and 0.15 ng/mL for cuIIa and cuIIb, respectively. The intra‐ and inter‐day precision was <11.5% for the LLOQs and each quality control level of the analytes, and accuracy was between ?9.1 and 7.6%. The extraction recoveries of the analytes and IS from rat plasma were all >87.1%. The method was fully validated and applied to compare the pharmacokinetic profiles of the two cucurbitacins in rat plasma after oral administration of H. amabilis extract between normal and indomethacin‐induced rats. Copyright © 2016 John Wiley & Sons, Ltd.     

Crystalline phase of Y_2O_3 :Eu particles generated in a substrate-free flame process

In this study, factors affecting the crystal structure of flame-synthesized Y 2 O 3 :Eu particles were inves- tigated, especially the particle size effect and its interaction with Eu doping concentration. Polydisperse Y 2 O 3 :Eu (size range 200 nm to 3 m) powder samples with Eu doping concentrations from 2.5 mol% to 25 mol% were generated in either H 2 /air or H 2 /O 2 substrate-free flames. The crystal structure of the powder samples was determined by powder X-ray diffraction (XRD), which was complemented...     

Achievable accuracy of parameter estimation for multidimensional NMR experiments

A fundamental issue in NMR spectroscopy is the estimation of parameters such as the Larmor frequencies of nuclei, J coupling constants, and relaxation rates. The Cramer-Rao lower bound provides a method to assess the best achievable accuracy of parameter estimates resulting from an unbiased estimation procedure. We show how the Cramer-Rao lower bound can be calculated for data obtained from multidimensional NMR experiments. The Cramer-Rao lower bound is compared to the variance of parameter estimates for simulated data using a least-squares estimation procedure. It is also shown how our results on the Cramer-Rao lower bound can be used to analyze whether an experimental design can be improved to provide experimental data which can result in parameter estimates with higher accuracy. The concept of nonuniform averaging in the indirect dimension is introduced and studied in connection with nonuniform sampling of the data.     

卢瑟福散射实验装置的研制

研制了一种鼎瑟福散的实验装置,并介绍了其实验结果,由于要用了步进电机和半导体探测器,该装置具有结构紧凑,操作简便等优点。     

快淬法制备La_(0.8)Ce_(0.2)Fe_(11.4)Si_(1.6)合金的磁熵变研究

为了探求La系磁熵变材料的短时退火工艺,利用两种方法制备了磁制冷材料La0.8Ce0.2Fe11.4Si1.6合金,其一为将电弧熔炼合金退火5天(样品A),其二为将合金利用铜模铸造方法得到快淬样品,再退火2 h(样品B)。X射线衍射表明,样品A和B主相为NaZn13相结构。通过对比发现,尽管样品A的最大磁熵变值大于样品B的,但样品B在制冷温区和制冷能力方面优于样品A。因此,快淬加短时间热处理可以大大节省时间和能量,是一种制备La0.8Ce0.2Fe11.4Si1.6磁制冷材料的高效且性能优越的方法。     

智能建筑通信平台集约系统研究——制冷设备信号的底层通信

文中为智能建筑设计了一个通信网络系统,以实现建筑物内的低温信号采集处理和信息交换。在已有硬件设施基础上,利用基于FPGA的SOC设计技术,通过需求分析、算法设计,再到硬件开发、系统集成,实现对低温信号的处理完善,使之从系统的底层开始,为动平衡过程的所有信息交互提供服务。该系统可以满足BACNet标准和LONMARK标准,为智能建筑自控提供一套有效的信息处理模式。     

准静态离散元方法和线性粘弹性问题的模拟

离散元方法是近年发展起来的一种新数值方法,但原则上只能用于动态问题。从静力平衡条件出发建立了离散元系统的准静态演化方程并证明了系数矩阵具有对称正定、稀疏、带状分布等特点,适用于“有效列”方法求解,该解法比高斯消去法节省更多的内存和机时。通过引入广义Maxwell体的元间作用模型建立起线性粘弹性材料准静态响应的离散元模拟方法。该方法独立于传统动态离散元方法,是传统动态离散元方法的拓展,可望在更多领域获得应用。     

多孔苯乙烯-二乙烯基苯共聚物微球的磺化及其对牛血清蛋白的吸附

在不同反应温度下对多孔苯乙烯-二乙烯基苯共聚物微球进行磺化亲水性修饰,采用扫描电镜与氮气吸附法,研究多孔微球的孔结构。结果显示,磺化反应修饰后,微球的孔容与比表面积变小,且随着磺化温度升高,比表面积与孔容递减。交换容量则随着磺化温度升高而递增。用牛血清蛋白作为模型蛋白质,研究了亲水性修饰后的多孔苯乙烯-二乙烯基苯共聚物微球对蛋白质大分子吸附性能的影响。实验结果表明,牛血清蛋白在磺化微球上的吸附主要由孔容与比表面积决定,孔容与比表面积越大,蛋白质吸附量也越大。吸附速率表现为疏水作用快于静电作用。吸附动力学研究表明,Kannan-Sundaram模型可较好地描述牛血清蛋白的吸附动力学行为。     

Magnesium oxide microspheres as a novel solid‐phase extraction sorbent for the determination of benzo[a]pyrene in environmental water samples

Magnesium oxide microspheres were developed as a novel SPE sorbent for the determination of benzo[a]pyrene (BaP), one of the most potent carcinogenic agents, in environmental water samples. The parameters controlling the extraction efficiency, such as elution volume, flow rate, pH values, and breakthrough volume, were investigated in detail. Considering the facile preparation and satisfying recovery, a corresponding analytical method has been developed to determine the concentration of BaP in real tap water, river water, and seawater. The recoveries for the spiked BaP were excellent (94–101%).