高效液相色谱-质谱-质谱法快速鉴定中药竹节香附的皂苷

应用反相高效液相色谱－电喷雾－质谱－质谱（RP－HPLC－ESI－MS－MS）方法对竹节香附皂苷提取物的化学成分进行分析,通过一步分析可以同时分离并鉴定出竹节香附中的竹节香附皂苷R2,R3,R6,R7,R8和R9等6种有效成分,同时也发现一些本药材中原来没有报道的成分,本研究结果为竹节香附及其相关药品有效成分分析和鉴定提供一种快速鉴定方法。     

硫酸皮肤素寡糖的分离与制备

利用软骨素酶ABC（Chondroitinase ABC,EC4.2.2.4)对硫酸皮肤素（Dermatan Sulfate,DS)进行控制降解。对得到的混合寡糖首先采用低压凝胶渗透色谱（LPGPC）进行分级,然后对每一组分再利用强阴离子交换高压液相色谱（SAX－HPLC）进行分离,最终制备出聚合度为2,4,6,8,10,12的寡糖纯品。寡糖纯度采用SAX－HPLC,毛细管电泳（CE）以及聚丙烯酰胺凝胶电泳（PAGE）进行检验,结构采用电喷雾离子化质谱（ESI－MS）以及核磁共振波谱（NMR）技术确定。     

利用氧化反应合成3—羟基—4—芳基—5—（1—苯基—5—甲基—1，2，3—三唑—4—基）—1，2，4—三唑衍生物的新方法

采用不同的氧化剂对ω[5-（1－苯基－5－甲基－1,2,3－三唑－4－基）－4－芳基－1,2,4－三唑－3－硫基]－ω－（1H－1,2,4－三唑－1－基）苯乙酮进行了氧化,结果发现KMnO4作为氧化剂时,氧化产物十分复杂,难于分离,而H2O2－AcOH及间氯过氧苯甲酸（MCPBA）又不能将其氧化,最后采用NaIO4作为氧化剂时没有得到相应的砜或亚砜而意外得到3－羟基－4－芳基－5－（1－苯基－5－甲基－1,2,3－三唑－4－基）－1,2,4－三唑衍生物,化合物的结构经元素分析和波谱确证,并对其生成机理作了初步讨论。     

N，N′—对苯二胺基—二苄基—α—氨基—1，3，2—二氧磷杂环膦酸酯的合成及表征

由芳香醛，异丁醛，三氯化磷和乙醇为原料制得中间体5，5－二甲基－1，3，2－二氧磷杂环乙烷－2－氧（DPDO），用DPDO与由芳醛和对苯二胺缩合制得的席夫碱（SB）经Pudovik加成反应，合成了系列膨胀型阻燃剂N，N′－对苯二胺基－二苄基－α－氨基－1，3，2－二氧磷杂环磷酸酯（A1－A12），并用IR，NMR，MS等对化合物进行了表征。     

十六烷基三甲基铵C60盐的合成和性质

采用钠萘还原剂制备C60负一阶离子，计量易控制、方法简便，利用复分解反应首次全成了十六烷三甲基铵的C60盐，产物经紫外可见－近红外光谱（V－NIR）、红外光谱(IR）、电喷雾电离质谱（ESI－MS）表征，研究了其电子顺磁共振谱（ESR）性质和被空气氧化的过程。     

南海海洋真菌Hypoxylon oceanicurm的代谢产物

对中国南海海洋真菌Hypoxylon oceanicurm（326号）的代谢产物进行研究,共分离得到8个化合物A－H,其中,8－羟基－9－酮－7（11）雅槛蓝烯－12,8－交酯（A）为新的倍半萜内酯化合物,它们的结构通过IR,FAB－MS,NMR（2DNMR）及元素分析数据得到确定。     

1—（3—吡啶甲酰基）—4—芳酰基硫脲类化合物的合成

报道了1－（3－吡啶甲酰基）－4－芳酰氨基硫脲类化合物的合成及鉴定。以烟酸和取代苯甲酸为起始原料,合成了一系列分子中含吡啶基团的芳酰氨基硫脲,经元素分析,IR光谱,^1H NMR谱和MS谱分析,确定了这类化合物的结构。     

一种DNA标记配体S—Acetyl—NHS—MAG3的合成研究

报导了S－乙酰基－硫基乙酸N－羟基丁二酰亚胺酯（SATA）,S－乙酰基－巯基乙酸三甘氨酸（S－Acetyl-MAG3),S-乙酰基－巯基乙酸三甘氨酸N－羟基丁二酰亚胺酯（S－Aectyl-NHS-MAG3)的合成方法,用IR和亚胺（DCC）的二氯甲烷溶液中,在40－50℃下反应24h得到S－乙酰基－巯基乙酸三甘氨酸N－羟基于二酰亚胺酯（S－Acetyl-NHS-MAG3) 的产率较高,副产物较少,分离提纯容易。     

双氯乙酰基二苯并—18—冠—6的合成

以多聚磷酸（PPA）为催化剂和反应溶剂,氯乙酸为酰化剂,对二苯并－18－冠－6进行酰化,成功地合成了双氯乙酰取代二苯并－18－冠－6,产物由IR,MS和元素分析鉴定了其结构。     

由ET反应制备5（6）—羟基—2—烷基—1，4—二甲氧基苯

通过单电子转移（ET）反应间接制备了5（6）-羧基-2-烷基-1，4-二甲氧基苯，通过2-烷基-1，4-二甲氧基苯（1）与过氧化二对硝基苯甲酰（2）的电子转移反应，在苯环上引入芳酰氧基；然后在温和条件下水解，可得到互为位置异构体的两种稀有酚3和4。用∧1HNMR、IR、MS分别表征了化合物的结构，反应机理研究发现，反应物2在1存在条件下，其分解速度急剧加快；用顺磁共振技术检测到了反应过程中产生的阳离子基信号，证明反应物1和2的反应是单电子转移反应，该反应条件温和，产率较高，产物易于分离纯化，是一种制备该类酚的简易方法。     

Markedness and its Interpretation in Language Use

Language markedness is a common phenomenon in languages, and is reflected from hearing, vision and sense, i.e. the variation in the three aspects such as phonology, morphology and semantics. This paper focuses on the interpretation of markedness in language use following the three perspectives, i.e. pragmatic interpretation, psychological interpretation and cognitive interpretation, with an aim to define the function of markedness.     

低渗透非均质砂岩油藏启动压力梯度研究

理论推导与室内实验相结合,建立了低渗透非均质砂岩油藏启动压力梯度确定方法。首先借助油藏流场与电场相似的原理,推导了非均质砂岩油藏启动压力梯度计算公式。其次基于稳定流实验方法,建立了非均质砂岩油藏启动压力梯度测试方法。结果表明:低渗透非均质砂岩油藏的启动压力梯度确定遵循两个等效原则。平面非均质油藏的启动压力梯度等于各级渗透率段的启动压力梯度关于长度的加权平均;纵向非均质油藏的启动压力梯度等于各渗透率层的启动压力梯度关于渗透率与渗流面积乘积的加权平均。研究成果可用于有效指导低渗透非均质砂岩油藏的合理井距确定,促进该类油藏的高效开发。     

On Tragic Consciousness In The Works By Ernest Hemingway

As an American modern novelist who were famous in the literary world, Hemingway was not a person who always followed the trend but a sharp observer. At the same time, he was a tragedy maestro, he paid great attention on existence, fate and end-result. The dramatis personae's tragedy of his works was an extreme limit by all means tragedy on the meaning of fearless challenge that failed. The beauty of tragedy was not produced on the destruction of life, but now this kind of value was in the impact activity. They performed for the reader about the tragedy on challenging for the limit and the death.     

Achieving Unusual States of Matter Under High Pressure

正The periodicity of the elements and the non-reactivity of the inner-shell electrons are two related principles of chemistry,rooted in the atomic shell structure.Within compounds,Group I elements,for example,invariably assume the+1 oxidation state,and their chemical properties differ completely from those of the p-block elements.These general rules govern our understanding of chemical structures and reactions.Using first principles calcula-     

Exchange-Correlation and Electronic Excitation Energies from Pairing Matrix Fluctuations

We have developed an adiabatic connection to formulate the ground-state exchange-correlation energy in terms of pairing matrix linear fluctuations.This formulation of the exchange-correlation energy opens a new channel for density functional approximations based on the many-body perturbation theory.We illustrate the potential of such approaches with an approximation based on the particle-particle Random Phase Approximation(pp-RPA).This re-     

Density Functional Theory for the Response of Periodic Systems to Electric Fields Based on the Vector Potential Approach

正The electronic and nuclear(structural/vibrational)response of 1D-3D nanoscale systems to electric fields gives rise to a host of optical,mechanical,spectral,etc.properties that are of high theoretical and applied interest.Due to the computational difficulty of treating such large systems it is convenient to model them as infinite and periodic(at least,in first approximation).The fundamental theoretical/computational problem in doing so is that     

On the Thermodynamic Limit for Responses to Static Electromagnetic Fields

For molecular systems,the quantum-mechanical treatment of their responses to static electromagnetic fields usually employs a scalar-potential treatment of the electric field and a vector-potential treatment of the magnetic field.Although the potential for each field separately is associated with the choice of an(unphysical)origin,the precise choice of the origin for the electrostatic field has little consequences for the results.This is different for the     

An affordable accurate evaluation of the binding conformations predicted by molecular docking studies in bio-system

Franck-Condon factors bridge the gap between theoretical modeling and experimental observations for molecular electronic spectroscopy and electron transfer.Under the displaced harmonic oscillator approximation,multidimensional Franck-Condon factors are decomposed into a product of many one-dimensional(1D)Franck-Condon(FC)factors,and each 1D-FC factor is associated with one Huang-Rhys factor that determines the leading contribution of     

Call for Papers

<正>"The Journal of Shanghai Normal University:Mathematics"is published by Shanghai Normal University as regular issues of The Journal of Shanghai Normal University each year from 2014 in English.The editors-in-chief of the issues are professors Yuhao Cong and Maoan Han.The Journal of Shanghai Normal University was started in 1958 with     

Journal of Donghua University ( English Edition) Contents of Volume 31

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