超临界流体萃取-胶束电动毛细管色谱法分离测定大黄中蒽醌类组分的含量

采用ＳＴＥ－ＭＥＣＣ法分离测定大黄中的芦荟大黄素，大黄素和大黄酸。萃取条件为压 力４１．４ＭＰａ，温度５０℃，改性剂量０．４ｍＬ。被测组分在１０ｍｉｎ得到全部分离。本法准确、简 便、快速、结果令人满意。     

非晶态镍磷—镍钨磷双层组合镀层的耐蚀性能研究

本文对比研究了镍磷镀层、镍钨磷镀层及非晶态镍磷和镍钨磷双层组合镀层的耐蚀性能，分别进行了各种镀层的浸渍腐蚀实验，镀层的Ｘ射线衍射图象、镀层的扫描电镜图象、以及在工厂实际的腐蚀环境里进行的腐蚀实验。实验结果表明镍磷及镍钨磷双层组合镀层的耐 性优于镍磷镀层、镍钨磷镀层的耐蚀性。     

Intein-mediated biotinylation of proteins and its application in a protein microarray

We report here the first example using an intein-mediated expression system to generate biotinylated proteins suitable for immobilization onto avidin-functionalized glass slides. With this novel array, proteins are site-specifically immobilized on the glass surface and are able to retain their native activity. The advantage of the avidin/biotin linkage over his-tag/Ni-NTA strategies for protein immobilization is highlighted by its ability to withstand a variety of chemical conditions, which makes this new protein array compatible with most biological assays.     

Identification of the function of gene lndM2 encoding a bifunctional oxygenase-reductase involved in the biosynthesis of the antitumor antibiotic landomycin E by Streptomyces globisporus 1912 supports the originally assigned structure for landomycinone

The angucycline antibiotic family of the landomycins displays potent antitumor activity. To elucidate early post polyketide synthase (PKS) tailoring steps of the landomycin E biosynthetic pathway in Streptomyces globisporus 1912, the mutant S. globisporus M12 was prepared through gene replacement experiment of lndM2. It encodes an enzyme with putative oxygenase and reductase domains, according to sequencing of the gene and its counterpart lanM2 from S. cyanogenus S136 landomycin A biosynthetic gene cluster. The isolation of the novel shunt products 11-hydroxytetrangomycin and 4-hydroxytetrangomycin along with the well-known angucyclines tetrangomycin and tetrangulol from the culture of S. globisporus M12 provides evidence for the involvement of lndM2 in the early biosynthetic pathway of the landomycins, in particular in the formation of the alicyclic 6-hydroxy function of the landomycin aglycon. We therefore propose LndM2 to be responsible for both hydroxylation of the 6-position and its subsequent reduction. These reactions are necessary before the glycosylation reactions can occur. The results are in agreement with the originally published structure of landomycin but do not support the recently suggested revised structure.     

The triplet channel in the photodissociation of ozone in the Hartley band: classical trajectory surface hopping analysis

The triplet channel in the photodissociation of ozone in the Hartley band, O3 + hv-->O(3P) + O2(3sigma), is investigated by means of a classical trajectory surface hopping method using ab initio diabatic potential energy surfaces for the B and the R states. Because of the strong recoil in the R state along the breaking O-O bond, O2(3sigma) is produced with a high rotational energy. The nonadiabatic transition probability depends markedly on the coordinate along the crossing seam. As a consequence a unique correlation is found between the internuclear geometry at the crossing and the final vibrational state of O2(3sigma). The calculated distribution of the translational energy is in good accord with the measured distribution.     

星形支化聚苯乙烯模型化合物的合成及表征

本文用阴离子聚合方法,首先合成了线形‘活’的聚苯乙烯大分子阴离子,然后用二乙烯基苯为偶联成核剂,制备了十三个4-80臂较窄分子量分布的等臂长规则星形支化聚苯乙烯的模型化合物,并用GPC—粘度计联用装置对之进行了表征。     

生物质快速热解制备液体燃料

本文回顾了生物质快速热解液化技术的国内外研究现状,重点叙述了初级生物油的化学组成和燃料性质,指出生物油是一种复杂的含氧有机混合物,具有水分含量高、氧含量高、热值低、酸含量高、安定性差和化石燃油不互溶等独特的性质;针对这些性质,介绍了几种常用的生物油精制提炼方法,包括催化裂解、催化加氢、高温热解气过滤、添加助剂、催化酯化、柴油乳化以及制备富氢合成气与费托合成,并分析了各种精制技术发展的关键问题。     

Reversed-phase liquid chromatography of proteins and peptides using multimodal copolymer-encapsulated silica

Multimodal copolymer-encapsulated particles for liquid chromatography were prepared by bonding 1-octadecene and unsaturated carboxylic acids on silica particles (5 microm diameter, 300 A pores) for liquid chromatography of proteins. These multimodal copolymer-encapsulated particles can provide both hydrophobic and hydrogen bonding interactions with polar compounds. The chromatographic performance of these multimodal copolymer-encapsulated particles for peptide and protein separations was evaluated under reversed-phase conditions. Compared with typical C8-bonded silica, polymer-encapsulated particles were more stable in acidic mobile phases and provided better recoveries, especially for large proteins (Mr>0.5 x 10(6)). Totally hydrophobic polymer-encapsulated particles were found to produce broad peaks for proteins, and significant improvements were observed by introducing hydrophilic groups (-COOH) onto the polymer-encapsulated surface to form a multimodal phase. For the reversed-phase liquid chromatography of peptides and proteins, improved selectivity and increased solute retention were found using the multimodal polymer-encapsulated particles. More peaks were resolved for the separation of complex peptide mixtures such as protein digests using the multimodal polymer-encapsulated particles as compared to totally hydrophobic polymer-encapsulated particles.     

Determination of binding sites in carboplatin-bound cytochrome c using electrospray ionization mass spectrometry and tandem mass spectrometry

Interaction of carboplatin with cytochrome c (Cyt. c) has been investigated by electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry (MS/MS). ESI-MS studies revealed that the ring-opened adducts of carboplatin with Cyt. c were formed in the stoichiometric ratio of 1:1 and 2:1 at pH 5.0 and 37 degrees C and in the stoichiometric ratio of 1:1 only at pH 7.0 and 37 degrees C. It was also found that Cyt. c could be cleaved by carboplatin at pH 2.5 and 50 degrees C. The cleaved fragments of Cyt. c were determined by ESI-MS and MS/MS analysis to be Glu66 approximately Met80, Ac-Gly01 approximately Met65, Glu66 approximately Glu104, Ac-Gly01 approximately Met80 and Ile81 approximately Glu104. The carboplatin prefers to anchor to Met65 first, then to Met80. To further confirm the binding site of Met, AcMet-Gly was used as the model molecule to investigate its interaction with carboplatin and its hydrolysis reaction. On the basis of species detected during the reaction monitored by ESI-MS, a possible pathway of the cleavage reaction was proposed.     

Preparation and thermal decomposition study of pyridinedicarboxylate intercalated layered double hydroxides

Supramolecular 2,3- and 2,5-pyridinedicarboxylate (PDC) intercalated ZnAl-layered double hydroxides (2,3- and 2,5-PDC–ZnAl–LDHs) have been prepared by ion exchange method. The structure and composition of the intercalated materials have been studied by X-ray diffraction (XRD) and inductively coupled plasma emission spectroscopy (ICP). The study indicates that the 2,3-PDC and 2,5-PDC anions are accommodated as interdigitated bilayer and monolayer arrangement respectively between the sheets of LDHs. Furthermore, their thermal decomposition processes were studied by the use of in situ high temperature X-ray diffraction (HT-XRD), and the combined technique of thermogravimetry-differential thermal analysis-mass spectrometry (TG-DTA-MS) under N2 atmosphere. Based on the comparison study on the temperatures of both decarboxylation and complete decomposition of interlayer PDC, it can be concluded that 2,5-PDC–ZnAl–LDHs has higher thermal stability than that of 2,3-PDC–ZnAl–LDHs.