Gilmicolin and Mycorrhizinol,Two New Metabolites of Gilmaniella humicolaBARRON

The structure of gilmicolin and mycorrhizinol, two new metabolites isolated from culture filtrates of Gilmaniella humicola BARRON , have been shown to be 3 and 15 respectively by spectral and chemical studies. The X-ray analysis of gilmicolin ( 3 ) is also reported.     

酞菁氧钛的合成及晶型转化

酞菁氧钛以联环己烷为溶剂，以邻苯二脂及四氯化钛直接反应生成。其优点是便于分离及纯化。同时对各晶型的获得及晶型间的相互转化进行了研究，并以Ｘ－射线粉末衍射及ＦＴ－ＩＲ进行了表征，并记录了不同晶型的酞菁氧钛在室温硫化硅橡胶中的吸收光谱。     

Gram-scale synthesis of (-)-epibatidine

[reaction: see text] A gram-scale approach toward (-)-epibatidine (1, naturally occurring enantiomer), a novel class of amphibian alkaloid, has been developed from readily available starting materials using mild and easily controlled reactions. The entire synthetic route is straightforward and convenient for gram-scale synthesis.     

Chromatographic molecular recognition for catechol-related compounds using thiacalix[4]arene as an effective selector

Thiacalix[4]arene (5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrahydroxy-2,8,14,20-tetrathiacalix[4]arene) is an amphiphilic molecule comprising four p-tert-butylphenol-like groups ortho-linked by single sulfur atoms. This molecule has a high electron density area owing to the close proximity of the hydroxyl groups and sulfur atoms. We studied the applicability of this interesting compound as a selector for high-performance liquid chromatography (HPLC) thereby presumably exploiting this feature. Firstly, uniformly sized polymer particles were prepared by using a multi-step swelling and polymerization method with ethylene glycol dimethacrylate (EDMA) as a cross-linker. Methacrylic acid (MAA) was introduced onto the surface of the resulting polymer particles through a new modification method. Thiacalix[4]arene was chemically bonded through the MAA group by using 1,4-dibromobutane as a spacer to reduce steric hindrance around the MAA and the polymer particle itself. The performance of the prepared polymer-based thiacalix[4]arene-modified stationary phase was evaluated with HPLC. Specific chromatographic retention behavior was observed for catechol relative to positional isomers of xylene, cresol, and benzene-diol. Catecholamine and catechol showed specific chromatographic retention behavior.     

批量离子交换层析和凝胶过滤层析在类人胶原蛋白I纯化中的应用

研究了利用批量离子交换层析与凝胶过滤层析相结合的方法纯化类人胶原蛋白I的最佳条件。分别考察了不同离子交换树脂、缓冲溶液pH、离子强度、进料蛋白浓度对批量离子交换的影响,以及不同凝胶过滤介质对凝胶过滤层析的影响。结果表明,采用阴离子交换树脂DEAE52吸附杂蛋白,缓冲液pH为7.0,NaCl浓度为0.2mol/L,进料蛋白浓度为40mg/mL,并采用凝胶过滤介质SephadexG-100进一步纯化后,类人胶原蛋白I的纯度可达到98.2%,总纯化倍数为3.1,总回收率为80.6%。SDS-PAGE分子量分析和N末端氨基酸序列分析均表明纯化后的类人胶原蛋白I与基因设计一致。     

流动注射分光光度法测定水体总磷

提出了一种单通道紫外消解流动注射比色分析法，能快速测定水样中总磷。实验采用了微量恒流混合泵、新型的细长型高灵敏度流通池及紫外消解器、液流分配阀、恒流瓶等FIA装置，并使用工业编程控制器和智能触摸屏进行控制和计算，使操作更为方便。此法分析时间短，测量范围宽，精度高，适合于各种水体的测定。     

A chiral 28-membered macrocycle with symmetry and structure similar to that of trans-cyclooctene

[reaction: see text] A bridged N,N-di(aryl)-1,2,4,5-benzenediimide was synthesized in which restricted rotation led to two diasteriomeric conformations at room temperature. The more stable syn-macrocycle is achiral, whereas the strained anti-macrocycle possesses planar chirality similar to that of trans-cyclooctene. The structure was characterized by X-ray crystallography, and the enantiomers were resolved by chiral chromatography.     

Recognition of chiral catechols using oxo-titanium phthalocyanine

Oxo-titanium phthalocyanine (TiOPc) derivatives of catechin and hematoxylin (natural ortho-diol type chiral compounds) have been prepared and characterized by spectral and chromatographic techniques. It is demonstrated that the TiOPc unit is an excellent template for chiral recognition through its isolated Q-transitions. The formation of a helical dimeric complex with hematoxylin induces strong CD-activity in the Q-band region. Ab initio geometry optimizations were combined with a Kuhn-Kirkwood coupled-oscillator mechanism to obtain the absolute configuration of hematoxylin. In addition, it is shown that the described chiroptical recognition method is sensitive to slight conformational changes.     

Gilmaniellin and Dechlorogilmaniellin,Two Novel Dimeric Oxaphenalenones

The structure and configuration of gilmaniellin, a metabolite of Gilmaniella humicola BARRON , has been shown to be 2 by X-ray analysis. By comparison of spectral data structure 1 has been assigned to dechlorogilmaniellin.     

卟啉超分子化合物在分子器件中的应用

分子电子器件已成为近年来的一个研究热点，卟啉类化合物因为光敏性好、性能稳定、易于修饰等优点成为分子器件研究的理想模型化合物。本文着重介绍了它在分子器件中的最新应用进展。