Synthesis and biological evaluation of 6-oxa-nor-tropane glycomimetics as glycosidase inhibitors

The preparation of polyhydroxylated 6-oxa-nor-tropane glycomimetics structurally related to the glycosidase inhibitor family of the calystegines is reported. The synthetic strategy involves the furanose→piperidine rearrangement of 5-deoxy-5-ureido-l-idose precursors, followed by intramolecular glycosylation involving the primary hydroxyl group. Inversion of the configuration at C-3 in the resulting 6-oxa-(+)-calystegine B₂ analogue allows accessing the elusive 3-epi-6-oxa-(+)-calystegine B₂ skeleton. Acid-catalyzed opening of the nor-tropane bicycle was observed, however, which could be avoided by careful neutralization of the reaction mixture. The inhibition results suggest that (+)-calystegine B₂ derivatives and the corresponding C-3 epimers can be seen as glucomimetics and galactomimetics, respectively, pointing to a 1-azasugar mode of action for this family of alkaloids.     

纳米晶Y_2SiO_5∶Eu的浓度猝灭研究

报道了分别用溶胶－凝胶法合成的Ｙ２ＳｉＯ５∶Ｅｕ纳米晶和用高温固相法合成常规尺度的Ｙ２ＳｉＯ５∶Ｅｕ材料的光致发光光谱和猝灭浓度的实验研究．结果表明：纳米Ｙ２－ｘＥｕｘＳｉＯ５比常规尺度的Ｙ２－ｘＥｕｘＳｉＯ５有更高的猝灭浓度和更高的发光亮度．理论分析认为这是由于在纳米材料中能量共振传递被阻断和猝灭中心在各个纳米晶内分布的涨落造成的．这个结果为高亮度的Ｙ２ＳｉＯ５∶Ｅｕ纳米材料的实际开发应用展示了广阔前景．     

XPS investigation of LPE garnet films

XPS spectra of YIG, YIG:Bi, YIG:Ca and YIG:Co(Ge, Ca) epitaxial garnet films were measured at room temperature. The positions of the main iron, yttrium, oxygen, bismuth, cobalt and lead spectral lines were determined and their changes with the surface treatments were investigated. It was found that divalent and trivalent states of iron and cobalt ions can be resolved, the chemical shifts being in oposite directions.The authors would like to thank Dr. J. imová for careful EPMA analysis of the samples.     

Conditioning of industrial waste in cement matrix

Results are presented of a series of experimental tests performed to determine the influence of matrix characteristics on the leaching mechanism of copper aluminium oxychloride immobilized into cement matrices. The objective of this research was to investigate the leaching mechanism of copper as a constituent of copper aluminium oxychloride (CAOX).     

聚丙烯腈热处理的反应机理

本文作者将聚丙烧腈样品分别在200°,250℃……的真空和空气中,以及在180°, 200℃……的氨气中,以逐步升温的方式进行热处理。在每一阶段处理的前后,对样品和产物的红外光谱、重量、它们在浓硫酸和冰醋酸中的溶解度、在浓硫酸中的紫外光谱、以及它们在冰醋酸回流抽提后所余残渣的红外光谱都进行了测量。提出了足以解释所有主要现象的反应机理,其中包括三个重要步骤的反应:(1)特征基团的产生,(2)分子内部的环化,(3)较高温度下的脱氨反应。从每个步骤反应的分析可以看出,热处理所得产物只能是含多核呲啶骈环不长、结构杂乱的高聚物。由于过去学者提出的反应机理只是根据部分实验结果考虑了分子内部环化的发生,而不可能发现到环化的必然中断,因此有些作者根据这机理所作关于产物的半导体电磁性能的解释是值得进一步研究的。     

Concentration and clean-up of trace hydrocarbons from atmospheric particulate matter

Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen (near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges (Supelclean ^tm LC-Silica SPE tubes and Sep-Pak^? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially important when aliphatic hydrocarbons concentrations are lower than 1 μg mL⁻¹. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples.     

Pu（^7Fg）＋H2（X^1∑g^＋,0,0）的分子反应动力学

基于PuH_2分子基态(X~7A_1)的分析势能函数，用准经典的Monte-Carlo轨线法 对Pu(~7Fg)+H_2(X~1∑_g~+，0，0)的分子反应动力学过程进行了计算。结果表明 ：Pu(~7F_g)与H_2(X~1∑_g~+，0，0)碰撞是弹性碰撞。     

A comparative study of several HPLC methods for determining free amino acid profiles in honey

A study of the viability of three derivatizing reagents for obtaining amino acid profiles in honey through high performance liquid chromatography (HPLC) is presented. A method using diode array detection based on a reaction with diethyl ethoxymethylene malonate (DEMM) and two other methods using fluorescence detection based on derivatization with fluorenylmethyl chloroformate (FMOC-Cl) and 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) have been developed. The three methods yield detection limits close to the ppb level, but vary in relation to other analytical characteristics. The use of methyl chloroformate derivatives allows the profile to be obtained with the greatest sensitivity within a short time frame. On applying such methods to honey samples of diverse botanical origin, we observe that the proline values obtained are always lower than those found using the official spectrophotometric method, thereby underlining the advisability of using HPLC methods to reduce uncertainty in these results.