Separation and identification of multiple constituents in Xiao Chai Hu Decoction (Sho‐saiko‐to) by bioactivity‐guided fractionation combined with LC‐ESI‐QTOFMS/MS

Xiao Chai Hu Decoction (XCHD), named Sho‐saiko‐to in Japanese, is a well‐known traditional Chinese medicine formula used in Asia. However, the characterization methods used in the past have lacked sensitivity and the nature of the active constituents of XCHD remains unclear. This study was carried out to establish the hyphenated method of bioactivity‐guided fractionation and liquid chromatography coupled with electrospray ionization quadrupole time‐of‐flight mass spectrometry (LC‐ESI‐QTOFMS/MS) in order to identify the major bioactive constituents of XCHD. D101 macroporous resin was used to separate and enrich the material base into four fractions, XCHD‐1, XCHD‐2, XCHD‐3 and XCHD‐4. Each fraction was then evaluated for its antidepressant effect using depression‐related parameters. An LC‐ESI‐QTOFMS/MS method in both positive and negative ion mode was also applied for separation and identification of the biological active fractions of XCHD. As a result, 79 compounds including polysaccharides, flavonoids, saikosaponins, ginsenosides, licoricesaponins and gingerols were detected, 69 of them were identified or tentatively characterized. Based on our preliminary characterization investigations, polysaccharides, gingerols and flavonoids in XCHD may contribute to the antidepressant effect of XCHD. In conclusion, the hyphenated method of bioactivity‐guided fractionation and LC‐ESI‐QTOFMS/MS was meaningful for the isolation and preliminary identification of the biological active components in complex matrices of traditional Chinese medicine. Copyright © 2014 John Wiley & Sons, Ltd.     

合成盐酸芬戈莫德的工艺改进

以溴苯为原料,经Wurtz偶联反应、Friedel-Crafts反应、烷基化反应等合成了免疫抑制剂盐酸芬戈莫德,总收率23.6%,其结构经1H NMR,IR和ESI-MS确证。     

DOPO衍生物改性碳纳米管的制备及对聚乳酸阻燃性能的影响

以含羧基的碳纳米管(CNT-COOH)和9,10-二氢-9-氧-10-磷杂菲-10-氧化物(DOPO)衍生物DOPO-NH₂为原料, 通过酰氯化反应、 缩合反应等制备了一种新型无机-有机杂化阻燃剂—DOPO衍生物改性碳纳米管(CNT-DOPO), 利用傅里叶变换红外光谱、 透射电子显微镜、 X射线光电子能谱及热重分析等对其结构进行表征并对有机物接枝率进行了定量测试. 结果表明, DOPO-NH₂成功接枝到碳纳米管上, 接枝率约为50%. 将CNT-COOH, DOPO-NH₂和CNT-DOPO以质量分数5%添加到聚乳酸(PLA)中制备阻燃PLA复合材料. 锥形量热测试结果表明, 与纯PLA相比, PLA/5CNT-COOH, PLA/5DOPO-NH₂和PLA/5CNT-DOPO 3种复合材料的热释放速率峰值分别下降46%, 3.4%和39.8%; 炭层形貌和结构分析表明, PLA/5CNT-DOPO的炭层石墨化程度最高, CNT-DOPO₂在凝聚相阻燃方面有明显的促进作用. 流变结果表明, 碳纳米管对黏弹转变影响很明显, PLA/5CNT-COOH和PLA/5CNT-DOPO基本上表现为弹性行为. 正是由于碳纳米管的存在, 使得PLA复合材料在低频区黏度增大, 并且在燃烧后期形成了连续致密的炭层, 有效降低了材料的热释放速率和烟释放.     

Decorating Covalent Organic Frameworks with High-density Chelate Groups for Uranium Extraction

The extraction of uranium from aqueous solution is highly desirable for sustaining the increasing demand for environmental safety and nuclear fuel. Herein, we report a strategy using a two-step covalent modification for the synthesis of covalent organic frameworks(COFs) with high-density amidoxime chelate groups at periphery. The introduction of dense amidoxime groups plays a pivotal role in uranium adsorption. The resulting COF exhibits strong affinity with the distribution coefficient of 5.2×10⁴ mL/g and a high adsorption capacity of 319.9 mg/g. The strategy could be expanded to identify and remove different contaminants by introducing special functional groups.     

在大学物理教学中应加强科学素养的案例剖析——纪念黄祖洽先生

通过具体的案例分析,探讨了在大学物理课程中对学生科学素养的培养.在大学物理课堂教学中引入批判性思维能力训练,激发学生发现科学问题,利用科学方法论解决问题.阐述了怎样更有效地在大学物理课堂教学中培育学生求真、求实、创新的科学精神.     

NaYF_4∶Yb~(3+),Tm~(3+)/CdSe纳米异质结构的近红外上转换发光性能

采用两步高温热分解法合成了纳米异质结构的Na YF4∶Yb3+,Tm3+/Cd Se。X射线衍射测试结果表明样品由纯六角相的Na YF4(β-Na YF4)和纤锌矿型Cd Se组成。980 nm激发的上转换光谱表明Na YF4∶Yb3+,Tm3+和Cd Se之间存在能量传递,Tm3+将Yb3+传递给它的能量部分地传递给Cd Se,被激发的Cd Se又将能量回传给Tm3+的相应能级,最终使得Na YF4∶Yb3+,Tm3+的紫外和蓝光发射完全消失,而797 nm的近红外发射大幅增强。Na YF4∶Yb3+,Tm3+/Cd Se纳米异质结构的激发光和发射光均处于生物组织的光学透过窗口(700~1 100 nm),对生物组织的光损伤小,在生物医学领域有很大的应用潜力。     

基于改进的剪切波变换和引导滤波的红外弱小目标背景抑制方法

由于传统的背景抑制方法没有充分利用信号的方向信息,使其不能有效区分背景边缘和红外弱小目标,从而造成背景抑制结果中有较多的背景泄露.针对上述问题,本文利用改进的剪切波变换和引导滤波,提出了一种新的背景抑制方法.首先,采用改进的剪切波变换对红外弱小目标图像进行多尺度和多方向分解,将图像分解得到不同的高频子带系数和低频子带系数;其次,利用目标信号与边缘在方向上的差异,采用自适应引导滤波对高频子带系数进行处理;再次,对分解后的低频子带系数和处理后的高频子带系数进行改进的剪切波逆变换,得到预测的背景图像;最后,将原图像与背景预测图像相减获得背景抑制且目标增强的红外图像.为了验证本文方法的有效性,采用多组实验对其进行验证,并与经典的Max-Median、TDLMS和Top-hat等方法作比较.多组实验结果均表明本文方法在主观视觉和客观评价指标方面均优于其它三种经典方法,可有效提高红外搜索跟踪系统对红外弱小目标的探测概率.     

时间测度链上一类具阻尼项的二阶非线性中立型动力方程的振荡准则（英文）

利用广义的Riccati变换及不等式分析技巧,获得时间测度链T上的一类具有阻尼项的二阶非线性变时滞泛函动力方程[A(t)Ф(yΔ(t))]Δ+b(t)Ф(yΔ(t))+P(t)F(Ф(x(δ(t))))=0振荡性的一些充分条件,这里y(t)=x(t)+B(t)g(x(τ(t)))且Ф(u)=u|u|λ-1(λ0).这些结果推广并改进了一些已知的结论,并通过例子来说明这些结果的重要性.     

Joint empirical likelihood confidence regions for a finite number of quantiles under strong mixing samples

In this paper, we obtain the joint empirical likelihood confidence regions for a finite number of quantiles under strong mixing samples. As an application of this result, the empirical likelihood confidence intervals for the difference of any two quantiles are also obtained.     

两类新的最优变重量光正交码

变重量光正交码用于光码分多址通信系统以满足不同服务质量用户需求.给出当u≥5为素数时,最优(16u,{3,5},1,{2/3,1/3))交重量光正交码的具体构造.同时证明了当u≥5为素数时,存在一个最优(25u,{3,4,5},1,{1/4,2/4,1/4})变重量光正交码.这将改进变重量光正交码的存在性结果.