Synthesis and characterization of β-cyclodextrin/fraxinellone inclusion complex and its influence on interaction with human serum albumin

Aqueous solubility is one of the key determinants in developing new chemical entities as drugs. In this study, to improve the solubility of fraxinellone, a novel β-cyclodextrin/fraxinellone inclusion complex was prepared and characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, X-ray diffraction, and elemental analysis. Moreover, the influence of inclusion of small molecule by cyclodextrins on its binding with transporter in human body is essential for drug development. For the first time, we report the interaction of fraxinellone and its inclusion complex with human serum albumin. Fluorescence quenching of albumin by fraxinellone and its inclusion complex is a static process through complex formation. The results indicated that β-cyclodextrin did not affect the binding force and site of fraxinellone to the protein. Furthermore, circular dichroism showed that both fraxinellone and its inclusion complex induced a significant change in the secondary structure of human serum albumin.     

Palladium catalyzed cross-dimerization of terminal acetylenes and acrylates

A palladium catalyzed oxidative cross-coupling reaction between terminal alkynes and acrylates was developed. In the presence of palladium catalyst and copper(II) acetate as oxidant, the cross dimerization products with were formed. This protocol provides a novel method to construct the tetrasubstituted functionalized alkenes.     

Rapid Construction of Structurally Diverse Quinolizidines,Indolizidines, and Their Analogues via Ruthenium‐Catalyzed Asymmetric Cascade Hydrogenation/Reductive Amination

A rapid construction of enantioenriched benzo‐fused quinolizidines, indolizidines, and their analogues by ruthenium‐catalyzed asymmetric cascade hydrogenation/reductive amination of quinolinyl‐ and quinoxalinyl‐containing ketones has been developed. This reaction proceeds under mild reaction conditions, affording chiral benzo‐fused aliphatic N‐heterocyclic compounds with structural diversity in good yields (up to 95 %) with excellent diastereoselectivity (up to >20:1 dr) and enantioselectivity (up to >99 % ee). Furthermore, this catalytic protocol is applicable to the formal synthesis of (+)‐gephyrotoxin.     

Combustion behavior and thermal stability of ethylene-vinyl acetate composites based on CaCO3-containing oil sludge and carbon black

CaCO₃-containing oil sludge (OS) is a by-product from petroleum industry, with great amount of production. Therefore, an effective processing methods for CaCO₃-containing OS is urgently needed. Herein, ethylene-vinyl acetate (EVA) composites based on CaCO₃-containing OS and carbon black (CB) were prepared by melt blending method. The combustion behavior and thermal stability of flame-retardant EVA/OS/CB composites were investigated by cone calorimeter test, limiting oxygen index (LOI), scanning electron microscopy (SEM), smoke density test (SDT), and thermogravimetry-Fourier infrared spectrometry. The heat release rate and smoke production rate of the ternary composites containing 3% CB significantly decreased compared with the EVA/OS composites and pure EVA. Moreover, addition of a certain amount of CB could evidently increase LOI values. The morphologies and structures of the residues, revealed by SEM, ascertained that a better carbonaceous protective layer was formed on the ternary composites than the EVA/OS composite. It was obtained from SDT that CB in the material could retard the smoke production with the application of the pilot flame. The EVA/OS/CB composites assumed a higher thermal stability than the EVA/OS composites and pure EVA.

     

Accurate discrimination of Gastrodia elata from different geographical origins using high‐performance liquid chromatography fingerprint combined with boosting partial least‐squares discriminant analysis

Gastrodia elata from different geographical origins varies in quality and pharmacological activity. This study focused on the classification and identification of Gastrodia elata from six producing areas using high‐performance liquid chromatography fingerprint combined with boosting partial least‐squares discriminant analysis. Before recognition analysis, a principal component analysis was applied to ascertain the discrimination possibility with high‐performance liquid chromatography fingerprints. And then, boosting partial least‐squares discriminant analysis and conventional partial least‐squares discriminant analysis were applied in this study. Experimental results indicated that the adaptive iteratively reweighted penalized least‐squares algorithm could eliminate the baseline drift of high‐performance liquid chromatography chromatograms effectively. And compared with partial least‐squares discriminant analysis, the total recognition rates using high‐performance liquid chromatography fingerprint combined with boosting partial least‐squares discriminant analysis for the calibration sets and prediction sets were improved from 94 to 100% and 86 to 97%, respectively. In conclusion, high‐performance liquid chromatography combined with boosting partial least‐squares discriminant analysis, which has such advantages as effective, specific, accurate, non‐polluting, has an edge for discrimination of traditional Chinese medicine from different geographical origins. And the proposed methodology is a useful tool to classify and identify Gastrodia elata from different geographical origins.     

结合傅里叶变换合成法设计均匀薄膜

基于傅里叶变换合成法的基本原理,合成了一个K9基底上的负滤光片,合成的渐变折射率薄膜具有期望光学特性,但实际制备难度很大,因此将其细分为足够多层离散折射率的均匀薄膜,由于实际薄膜材料种类有限,不能获得任意折射率膜层,鉴于两层高低折射率薄层可近似为一层中间折射率膜层的思想,将膜系转化成一个可实际制备的膜系结构:膜系采用ZrO2和SiO2两种膜料,膜层总数为183层,经单纯形调法优化后,膜层总厚度为7.09 μm,通带和截止带内平均透射比分别为97.56%和3.13%,其结果优于直接采用傅里叶方法合成的非均匀膜系,与期望透射比曲线吻合更好.说明通过这种思想设计任意光谱特性的膜系是可行的,也使傅里叶变换合成法设计的薄膜实际制备成为可能.     

Optical phonons in millerite (NiS) from single‐crystal polarized Raman spectroscopy

Although several fundamental physico‐chemical aspects of nickel sulfides have been studied in detail, particularly for millerite (nickel(II) monosulfide), the most common nickel sulfide mineral, no satisfactory investigation of optical vibrational modes has been reported previously. In this paper, we provide a definitive assignment of the optical phonons in millerite, investigated by polarized Raman spectroscopy on an oriented single crystal. The impact of the power of the incident laser beam on the spectra has also been investigated, revealing evidence for degradation in the quality of the spectra at sufficiently high laser power. Copyright © 2008 John Wiley & Sons, Ltd.     

富晶格位错的多孔铋纳米花高效电还原二氧化碳制甲酸盐※

二氧化碳转化已成为现今世界研究的热点. 本工作采用原位电化学转化的策略, 将简单溶剂热法合成的层状甲酸氧铋纳米花(BiOCOOH NFs)还原为带有大量晶格位错的多孔铋纳米花(p-Bi NFs). 研究结果表明, p-Bi NFs电催化二氧化碳转化为甲酸盐具有较小的过电位(436 mV). 在–1.8 V(相对饱和甘汞电极, vs. SCE)时, 甲酸盐的分电流密度(j_formate)高达24.4 mA•cm^-2, 法拉第效率(FE_formate)为96.7%, 且在超过500 mV的宽电位窗口内FE_formate超过90%, 并具有很好的稳定性. 该催化剂的高催化性能可归因于前驱体晶格坍塌和重构而形成特殊的多孔粗糙的微纳多级结构, 其表面富含晶格位错和缺陷等高本征活性位, 且具有较强的电子传递能力. 本研究为设计合成高性能的电催化二氧化碳还原产甲酸催化剂提供了新的思路.     

One-step synthesis of magnetic composite UiO-66/Fe3O4/GO for the removal of radioactive cesium ions

Journal of Radioanalytical and Nuclear Chemistry - In this study, the UiO-66/Fe3O4/GO composite was prepared by one step method for removal of cesium ions (Cs+) in water and exhibited excellent...