加压毛细管电色谱法高效分离分析葛根多糖中的单糖

葛根多糖具有抗氧化、抗肿瘤等众多生物活性,对葛根多糖进行单糖组成分析对其活性研究具有重要意义。该研究利用响应面分析法考察了超声辅助提取法中液料比、超声温度、超声时间和超声功率对葛根多糖提取率的交互影响,并拟合数据得到多元二次回归方程。同时建立了柱前衍生加压毛细管电色谱检测糖类的方法,对分离8种中性单糖的色谱条件进行了探索与优化,并将此方法应用于两种葛根实际样品的单糖组成测定。响应面分析结果表明,4个试验因素中,超声温度对两种葛根多糖提取率的影响程度最大,其次为液料比,超声时间和超声功率影响程度较小。结合软件预测分析得到的最佳条件及设备实际情况,确定葛根多糖的最佳提取工艺条件为：超声温度90℃,粉葛多糖液料比20 mL/g,柴葛多糖液料比40 mL/g,超声时间30 min,超声功率180 W。优化后的色谱分离条件为：采用Halo-2.7 μm核壳型C18填料毛细管色谱柱,以乙腈-50 mmol/L pH 4.1的醋酸铵水溶液（18：82,v/v）为流动相,在250 nm波长下检测,施加电压-20 kV。在此条件下可以实现24 min内对葡萄糖等8种中性单糖衍生物的快速分离,相比传统液相色谱方法大大提升了分离检测速度和分离柱效。方法学考察表明此方法具有较好的线性关系和良好的重复性。对实际样品分离鉴定表明,粉葛多糖主要由葡萄糖、甘露糖、鼠李糖和岩藻糖组成,4种单糖物质的量之比为1.00：0.16：0.14：0.07;柴葛多糖主要由葡萄糖和甘露糖组成,2种单糖物质的量之比为1.00：0.70。该研究为单糖化合物快速高效分离检测提供了新方法,并为葛根多糖单糖组成分析提供了参考。     

气相色谱-串联质谱法同时测定锂离子电池电解液中13种有机磷阻燃剂的含量

建立了一种可同时测定锂离子电池电解液中13种有机磷阻燃剂含量的气相色谱-串联质谱分析方法,以乙酸乙酯为萃取溶剂,超声萃取锂离子电池电解液中的有机磷阻燃剂,萃取液经浓缩、定容、过滤后进行气相色谱-串联质谱分析,外标法定量。结果显示,13种有机磷阻燃剂在一定浓度范围内线性良好,相关系数不低于0.999 3,方法的检出限(S/N=3)为0.3~30μg/kg,定量下限(S/N=10)为1~100μg/kg。在低、中、高3个加标水平下的平均回收率为80.4%~94.6%,相对标准偏差(RSD)为3.8%~10%。该方法简单快捷,灵敏度高,定量下限低,可满足锂离子电池电解液中有机磷阻燃剂含量日常检测需要。     

Heterometallic Feed Ratio-Dominated Oxygen Evolution Activity in Self-Supported Metal-Organic Framework Nanosheet Arrays Electrocatalyst

Developing earth-abundant, highly active and long-term durable electrocatalysts for oxygen evolution reaction (OER) is highly desirable and great challenging for large-scale industrial application of electrochemical water splitting. Herein, in-situ growth of uniform nanosheet arrays on nickel foam (NF) is hydrothermally achieved by varying feed ratios of Fe^III and Ni^II salts. The feed ratio of the two active metals has significantly dominated both the morphological and electronic structures of the resultant electrocatalysts, leading to feed ratio-dependent volcano-type OER activity. The optimized Fe_0.89Ni_0.11-BDC/NF exhibits the best OER performance, affording a low overpotential of 220 mV to drive a current density of 50 mA · cm^–2 with small Tafel slope of 44.8 mV · dec^–1 and long-lasting stability over 20 hours. The synergistic effect from the Fe^III and Ni^II species on both the morphological and electronic structure modulations have dramatically accelerated the reaction kinetics, responsible eventually for the enhanced OER activity. This work provides valuable information for nanostructured MOFs as efficient electrocatalysts.     

A Glycan Array‐Based Assay for the Identification and Characterization of Plant Glycosyltransferases

Growing plants with modified cell wall compositions is a promising strategy to improve resistance to pathogens, increase biomass digestibility, and tune other important properties. In order to alter biomass architecture, a detailed knowledge of cell wall structure and biosynthesis is a prerequisite. We report here a glycan array‐based assay for the high‐throughput identification and characterization of plant cell wall biosynthetic glycosyltransferases (GTs). We demonstrate that different heterologously expressed galactosyl‐, fucosyl‐, and xylosyltransferases can transfer azido‐functionalized sugar nucleotide donors to selected synthetic plant cell wall oligosaccharides on the array and that the transferred monosaccharides can be visualized “on chip” by a 1,3‐dipolar cycloaddition reaction with an alkynyl‐modified dye. The opportunity to simultaneously screen thousands of combinations of putative GTs, nucleotide sugar donors, and oligosaccharide acceptors will dramatically accelerate plant cell wall biosynthesis research.     

激光激发超声波的新方法研究

介绍了激光激发超声波的原理，分别给出了热弹机制和烧蚀机制下的纵波和剪切波理论波形；基于排列因子作用，提出了一种新型激光激发超声波的方法——激光定相位排列激发超声波，激光源经过定相位排列后，在某一方向上产生的超声波幅度比传统单一源产生的超声波幅度要强很多，采用此种方法，可实现对超声信号方向和强度的有效激发控制，对下一步的超声无损检测有非常重要的意义；结合实际给出了该方法的实现方式.     

Magnetic avalanches: Josephson, Bean, and Bak

Josephson junction arrays provide an ideal physical realization for studying the complex dynamics of the sort found in sandpile models. They provide a means of separately investigating the dual physical effects of nonlinearity and disorder, and hold promise as an example for establishing a rigorous connection between the governing differential equations and the corresponding cellular automaton.     

不同工艺下YAG:Ce3+荧光粉的超声共沉淀合成及表征

用共沉淀正滴及反滴工艺,以普通共沉淀及超声辅助共沉淀的方式制备了不同YAG∶Ce³⁺前驱体,并通过焙烧前驱体粉末合成了YAG∶Ce³⁺荧光粉。利用XRD、SEM、激光粒度分布仪及荧光分光光度计对所制备样品进行了表征。结果表明,所得样品均为纯相钇铝石榴石结构,反滴工艺下制得的YAG∶Ce³⁺荧光粉的发光强度高于正滴工艺下的同类样品。且相对于普通共沉淀来说,无论正滴还是反滴工艺,通过超声共沉淀方式制得的荧光粉样品均具有更均匀的晶粒粒径、更窄的粒径分布及更高的发光强度。     

Structural phase transition in ferroelectric fluorine polymers: X-ray diffraction and infrared/Raman spectroscopic study

The structural phase transition has been investigated by X-ray diffraction and infrared and Raman spectroscopic measurements for ferroelectric fluorine polymers, including poly(vinylidene fluoride) and its copolymers with trifluoroethylene or tetrafluoroethylene. One of the most characteristic features of this ferroelectric transition is the large conformational change of the molecular chains between the trans and gauche rotational isomers, quite different from the structural change observed generally in the usual ionic ferroelectric materials. The crystallization and transition behaviors depend sensitively on the monomer composition in the copolymers as well as on the sample preparation conditions. The roles of the optic and acoustic phonons in the ferroelectric phase transition have been discussed based on the temperature dependences of the far-infrared spectra and the ultrasonic velocity.     

Fabrication of two-dimensional colloidal arrays

We report the effective fabrication of two-dimensional (2D) arrays of submicron colloidal particles. These colloidal arrays are produced in thin layers of monodisperse colloid suspensions on flat surfaces of solids such as clean glass or cleaved mica. The process of colloid assembling includes two steps, nucleation and growth, similar to those found in crystallization in solution but each of the steps in detail progresses with different mechanisms. The nucleation process is initiated by a special kind of capillary force acting parallel to the surface. The growth is guided by a laminar flow of water to the crystals, which is driven by water evaporation from 2D arrays. What is distinguishable in the 2D assembling is its active nature governed by the forces and flows, making a contrast to the diffusive mechanism in ordinary crystallization. With this two-step mechanism, a domain of hexagonally packed colloidal array can grow with time. A large and uniform film of particle monolayer is, thus, formed in a short period, from several seconds up to several minutes depending on the conditions controlled.     

Investigations of Linearly Chirped Fiber Bragg Gratings for Time-Steered Array Antennas

The use of linearly chirped fiber Bragg gratings as dispersive delay line elements in optical true time-delay beamformers is investigated. Two different dispersive prism beamforming architectures are considered as is their impact on the grating specifications. Microwave double-sideband and single-sideband characterization is carried out on gratings suitable for both architectures with an emphasis on the group delay ripple of single and cascaded gratings. Results indicate that commercially available gratings are suitable for beamforming applications.