一种基于形成杂多核配合物的荧光增敏效应的研究（Ⅱ）──钴（Ⅱ）－7－（8－羟基－3，6－二磺基萘偶氮）－8－羟基喹啉－5－磺酸－硼（Ⅲ）三元体系的荧光性质及其分析应用

一种基于形成杂多核配合物的荧光增敏效应的研究（Ⅱ）──钴（Ⅱ）－７－（８－羟基－３，６－二磺基萘偶氮）－８－羟基喹啉－５－磺酸－硼（Ⅲ）三元体系的荧光性质及其分析应用熊国华，刘虹，俞英，黄坚锋（九江师范专科学校化学系，九江，３３２０００）（江西大学实...     

Selective functionalizations of 2-phenylpyridine: lactones upon organic versus organometallic activations

2-Phenylpyridine activated by chromium tricarbonyl reacts with bis(TMS) ketene acetals to give pyridine-substituted bicyclic γ-lactones. On the other hand, its reaction with the same acetals leads, upon activation with methylchloroformate, to dihydropyridines which can be oxidized to highly substituted, lactone-containing piperidines.     

溶剂热法制备Ag/TiO2纳米材料及其光催化性能

以乙醇为溶剂, 钛酸四丁酯为前驱体, 用溶剂热法制备了Ag表面修饰的负载型纳米二氧化钛光催化剂. 利用X射线衍射(XRD)、N₂吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、紫外-可见(UV-Vis)光谱等技术对其进行了系统的表征, 以亚甲基蓝(MB)溶液的脱色降解为模型反应, 考察了不同Ag含量样品的光催化性能. 结果表明: 用溶剂热法制备的样品中TiO₂皆为锐钛矿相, 金属Ag颗粒沉积在TiO₂表面, 粒径为2 nm左右, 比表面积较溶胶凝胶法制备的样品大大增加, 最高可达151.44 m²·g^-1; UV-Vis光谱和光催化实验表明: Ag修饰使TiO₂对光的吸收能力大大增强, 吸收带边红移至可见光区, 亚甲基蓝在该复合材料上的光催化降解反应遵循一级反应动力学模型; 溶剂热法制备样品的光催化性能明显好于溶胶凝胶法制备的样品, 在紫外光和可见光下, Ag摩尔分数为5%的样品表现出最佳的光催化活性.     

基质辅助激光解吸附飞行时间质谱分析缩合单宁的阳离子化问题

以单价金属离子Cs 和Na 作为离子化试剂,对3种缩合单宁进行基质辅助激光解吸附飞行时间(MALD I-TOF)质谱分析。加入Na 作为阳离子化试剂,能得到较高质量的质谱图。但由于实验通道中几乎不可能完全去除的K 的干扰而会高估棓儿茶酚/表棓儿茶酚单元的组成比例,从而影响对棓儿茶酚/表棓儿茶酚单元存在与否的判断;选择Cs 作为阳离子化试剂可以避免此问题,但在复杂的缩合单宁分析中,同样因为杂质离子Na 和K 的干扰而使得质谱图变得更复杂;未去离子处理直接对缩合单宁进行MALD I-TOF质谱分析与去离子并加入Cs 的处理比去离子并加入Na 能检测到更高聚合度的高聚物,检测到离子峰强度最高的聚合物随离子不同而不同。     

Mesoscopic simulation of the aggregation behavior of fluorinated surfactant in aqueous solution

The aggregation behavior of fluorinated surfactant in aqueous solution was investigated using dissipative particle dynamics (DPD) simulation method. Simulation results show that fluorinated surfactants behave mainly as their hydrocarbon analogues, having similar sequences of phases and aggregate structures, which are capable of building micelle, hexagonal phase and lamellar phase. But fluorinated surfactants also show interesting differences from hydrocarbon analogues, which can easily form hexagonal and lamellar structures with comparative little curvature. They can also form ellipsoid or rod-like micelles even in very low concentrations instead of spheroid ones. The dynamic aggregation behavior of fluorinated surfactants, as well as the comparison with hydrogenated ones, was also investigated.     

3-(D-葡萄糖-1-基)-6-芳基-7H-1，2，4-三唑并[3，4-b][1，3，4]噻二嗪类化合物的合成及波谱研究

ω-溴代芳香基乙酮与3-(D-葡萄糖-1-基)-4-氨基-5-巯基-1，2，4-三唑反应 合成了一系列新颖的3-(D-葡萄糖-1-基)-6-芳基-7H-1，2，4三唑并[3，4-b[1，3 ，4]噻二嗪．用元素分析，IR，NMR，MS对其结构进行了表征，研究了其NMR波谱特 征，并以^1H-^1H COSY，^13C-^1H COSY，COLOC二维NMR技术对其^1H NMR，^13C NMR的谱峰进行了全归属     

一系列新型三环二萜的合成与抗肿瘤活性研究

对活性天然产物(+)-7-deoxynimbidiol非对映异构体的外消旋体cis-(±)-7-deoxynimbidiol进行了合成和衍生, 共得到了8个新型三环二萜化合物; 对合成的新化合物进行了抗肿瘤活性的实验研究, 其中化合物5d对人体乳腺癌瘤株MCF7表现出了较强的抑制作用(IC50=7.49 μg/mL), 可能作为新型抗肿瘤药物先导化合物.     

指纹图谱法在参麦注射液质控中的应用

 中医药理论和实践要求综合评价中药的质量 ,指纹图谱法是对中药制剂进行综合宏观分析的可行手段之一 ,因此采用反相高效液相建立了参麦注射液的特征指纹图谱。条件 :Hypersil C18(4 6mmi d × 2 5 0mm ,5 μm)反相柱 ,流动相由水 (A)和乙腈 (B)组成 ,B的体积分数在 5 0min内由 5 %线性增长到 95 % ,流速为1 0mL/min ;紫外检测 ,波长为 2 0 2nm。 2 3个特征指纹峰与内标 (联苯 )的峰面积比作为指标 ,结合主成分分析 投影判别法比较了同一厂家不同批次产品和不同厂家同类产品的化学指纹差异。     

Design of a calcium-binding protein with desired structure in a cell adhesion molecule

Ca2+, "a signal of life and death", controls numerous cellular processes through interactions with proteins. An effective approach to understanding the role of Ca2+ is the design of a Ca2+-binding protein with predicted structural and functional properties. To design de novo Ca2+-binding sites in proteins is challenging due to the high coordination numbers and the incorporation of charged ligand residues, in addition to Ca2+-induced conformational change. Here, we demonstrate the successful design of a Ca2+-binding site in the non-Ca2+-binding cell adhesion protein CD2. This designed protein, Ca.CD2, exhibits selectivity for Ca2+ versus other di- and monovalent cations. In addition, La3+ (Kd 5.0 microM) and Tb3+ (Kd 6.6 microM) bind to the designed protein somewhat more tightly than does Ca2+ (Kd 1.4 mM). More interestingly, Ca.CD2 retains the native ability to associate with the natural target molecule. The solution structure reveals that Ca.CD2 binds Ca2+ at the intended site with the designed arrangement, which validates our general strategy for designing de novo Ca2+-binding proteins. The structural information also provides a close view of structural determinants that are necessary for a functional protein to accommodate the metal-binding site. This first success in designing Ca2+-binding proteins with desired structural and functional properties opens a new avenue in unveiling key determinants to Ca2+ binding, the mechanism of Ca2+ signaling, and Ca2+-dependent cell adhesion, while avoiding the complexities of the global conformational changes and cooperativity in natural Ca2+-binding proteins. It also represents a major achievement toward designing functional proteins controlled by Ca2+ binding.     

溶剂热法制备Ag/TiO2纳米材料及其光催化性能

以乙醇为溶剂, 钛酸四丁酯为前驱体, 用溶剂热法制备了Ag表面修饰的负载型纳米二氧化钛光催化剂. 利用X射线衍射(XRD)、N₂吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、紫外-可见(UV-Vis)光谱等技术对其进行了系统的表征, 以亚甲基蓝(MB)溶液的脱色降解为模型反应, 考察了不同Ag含量样品的光催化性能. 结果表明: 用溶剂热法制备的样品中TiO₂皆为锐钛矿相, 金属Ag颗粒沉积在TiO₂表面, 粒径为2 nm左右, 比表面积较溶胶凝胶法制备的样品大大增加, 最高可达151.44 m²·g^-1; UV-Vis光谱和光催化实验表明: Ag修饰使TiO₂对光的吸收能力大大增强, 吸收带边红移至可见光区, 亚甲基蓝在该复合材料上的光催化降解反应遵循一级反应动力学模型; 溶剂热法制备样品的光催化性能明显好于溶胶凝胶法制备的样品, 在紫外光和可见光下, Ag摩尔分数为5%的样品表现出最佳的光催化活性.