反相高效液相色谱法同时测定壮阳类保健品中达泊西汀和4种PDE5抑制剂

提出了反相高效液相色谱法同时测定壮阳类保健品中4种PDE5抑制剂和达泊西汀含量的方法。样品溶于水中,再加甲醇提取。分取10μL提取液进样,并用Inertsil ODS-SP色谱柱为分离柱和由(A)三乙胺-乙酸-水(8+4+988)混合液,(B)乙腈和(C)0.02%(φ)磷酸溶液三者按不同比例相混的混合液作流动相进行梯度淋洗和分离。在检测波长290nm处进行测定。他达那非的质量浓度在1.25~25.0mg·L-1范围内与其峰面积呈线性关系,其余4种化合物的质量浓度在5.0~100mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.05~0.2mg·L-1之间。加标回收率在94.1%~109%之间,测定值的相对标准偏差(n=6)均小于1.0%。     

Blue electroluminescence of a novel Zn~(2+)–β-diketone complex with a carbazole moiety

In this letter, a novel zinc complex of Zn(ECTFBD)2 was synthesized by an environment-friendly grinding technique in high yield. Its structure was confirmed by1H NMR, MS and EA. HECTFBD is 1-(9-ethyl-9Hcarbazol-3-yl)-4,4,4-trifluorobutane-1,3-dione. Zn(ECTFBD)2-based light-emitting devices were fabricated. The architecture of the devices was ITO/PEDOT(40 nm)/100 wt% PVK: 40 wt% OXD-7: x wt% Zn(ECTFBD)2(85 nm)/CsF(1.5 nm)/Al(100 nm), where x = 1, 5, and 10(relative to the mass of PVK and OXD-7). The three devices displayed blue emissions with peaks at 450, 458, and 460 nm, respectively. A maximum luminous efficiency of 0.86 cd/A and a luminance of 228 cd/m2were achieved by the 1 wt% doped device. So, we demonstrated further that Zn2+–b-diketone complexes can be effectively severed as a class of new electroluminescent materials. In addition, the thermal stability of Zn(ECTFBD)2 was tested and the UV–vis and photoluminescent behaviors of Zn(ECTFBD)2 in CH2 Cl2 were investigated.     

全印刷工艺制备聚合物OLED显示屏

详细探讨采用全印刷工艺,制备聚合物OLED显示屏的工艺流程和技术难点的克服。通过喷墨打印纳米银电子墨水制备金属阴极,完全避免了高温及真空工艺的使用。在显示屏制备过程中,我们成功研发由水/醇溶性共轭聚合物聚[9,9-二辛基芴-9,9-双(N,N-二甲基胺丙基)芴],与一种可固化的环氧树脂粘合剂共混形成的多功能缓冲层。此多功能缓冲层,一方面保护有机功能层,避免纳米阴电子墨水的侵蚀,另一方面提供必需的电子注入功能,使高功函银阴极可以有效地注入电子。通过研究表面能优化打印阴极的成型形貌,并克服工艺难点,所制得的96×3×64分辨率的单色和全彩色聚合物OLED显示屏无坏点/坏线,红、绿、蓝电流效率分别为0.62、4.38、0.93cd/A,色坐标分别为(0.63,0.37)、(0.39,0.57)、(0.18,0.16)。     

Allyl phthalazinone synthesis,polymerization and polymer properties

A phthalazinone monomer with an allyl group, i.e. 4-（3-allyl-4-hydroxyphenyl）phthalazin-1（2H）-one, was synthesized and then copolymerized with 4-（4-hydroxylphenyl）（2H）-phthalazin-1-one and 2,6- diflurobenzonitrile by means of aromatic nucleophilic polycondensation to provide a series of crosslinkable poly（aryl ether nitrile）s. The virgin copolymers exhibited good solubility in polar organic solvents with relative high molecular weights （Mw： 45,130-58,403, inherent viscosities： 0.58-0.75 dL/ g）. After cross-linking, the thermal stability and solvent resistance of the polymer increased.     

拉曼光谱技术在聚合物研究中的应用进展

拉曼光谱可以提供分子的振动信息,对于聚合物分子链的构象和链间的相互作用非常敏感,能够提供聚合物固体、薄膜或溶液的物理化学特性信息,如聚合物的结构单元、空间构型、晶态结构、分子链的物理构象或分子链子链和侧基在界面间或在各向异性材料中的排列等链取向信息等。因此拉曼光谱作为一种原位无损检测技术,其衍生出的表面增强拉曼光谱技术(Surface-enhanced Raman Scattering,SERS)、变温拉曼光谱技术、共焦显微拉曼光谱技术(Confocal Raman Microscopy,CRM)、拉曼Mapping成像技术和共振拉曼散射技术(Resonance Raman scattering,RRS)等,广泛应用于物理、化学和生物医学等领域。本文从拉曼光谱的基本理论基础、拉曼光谱技术及其在聚合物研究中的最新应用进展等方面进行综述,以探索扩展拉曼光谱技术在高分子物理与化学领域中许多问题,如分子链的构象结构、分子链的结晶行为、分子链的扩散运动和共混体系相态结构变化等方面的应用。     

Sulfur/carbon composites prepared with ordered porous carbon for Li-S battery cathode

Ordered porous cabon with a 2-D hexagonal structure,high specific surface area and large pore volume was synthesized through a twostep heating method using tri-block copolymer as template and phenolic resin as carbon precursor.The results indicated the electrochemical performance of the sulfur/carbon composites prepared with the ordered porous carbon was significantly affected by the pore structure of the carbon.Both the specific capacity and cycling stability of the sulfur/carbon composites were improved using the bimodal micro/meso-porous carbon frameworks with high surface area.Its initial discharge capacity can be as high as 1200 mAh·g~(-1) at a current density of 167.5 mA·g~(-1)The improved capacity retention was obtained during the cell cycling as well.     

Graphene oxide assisted facile hydrothermal synthesis of LiMn0.6Fe0.4PO4 nanoparticles as cathode material for lithium ion battery

Assisted by graphene oxide（GO）,nano-sized LiMn0.6Fe0.4PO4 with excellent electrochemical performance was prepared by a facile hydrothermal method as cathode material for lithium ion battery.SEM and TEM images indicate that the particle size of LiMn0.6Fe0.4PO4（S2）was about 80 nm in diameter.The discharge capacity of LiMn0.6Fe0.4PO4 nanoparticles was 140.3 mAh-g^1 in the first cycle.It showed that graphene oxide was able to restrict the growth of LiMn0.6Fe0.4PO4 and it in situ reduction of GO could improve the electrical conductivity of LiMn0.6Fe0.4PO4 material.     

一种萘并吡喃化合物的合成及其工艺研究

本文以4,4'-二甲氧基二苯甲酮、苯乙酮和呋喃甲醛为原料,采用新的路线,6步反应合成了一种新型萘并吡喃类化合物,借助核磁共振、质谱等检测手段对最终产物的结构进行了结构表征,并对其反应条件进行优化,提高了反应收率,最后应用紫外-可见吸收光谱对目标产物在不同溶剂中的光致变色性质进行了初步探索研究。     

Gene Cloning,Expression, and Characterization of an Exo-inulinase from Paenibacillus polymyxa ZJ-9

An inulinase-producing strain, Paenibacillus polymyxa ZJ-9, was isolated from natural sources to produce R,R-2,3-butanediol via one-step fermentation of raw inulin extracted from Jerusalem artichoke tubers. The inulinase gene from P. polymyxa ZJ-9 was cloned and overexpressed in Escherichia coli BL21 (DE3), and the purified recombinant inulinase was estimated to be approximately 56 kDa by both sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS–PAGE) and gel filtration chromatography. This result suggests that the active form of the inulinase is probably a monomer. Terminal hydrolysis fructose units from the inulin indicate that enzymes are exo-inulinase. The purified recombinant enzyme showed maximum activity at 25 °C and pH 6.0, which indicate its extreme suitability for industrial applications. Zn²⁺, Fe²⁺, and Mg²⁺ stimulated the activity of the purified enzyme, whereas Co²⁺, Cu²⁺, and Ni²⁺ inhibited enzyme activity. The K _m and V _max values for inulin hydrolysis were 1.72 mM and 21.69 μmol min^?1 mg^?1 protein, respectively. The same parameters toward sucrose were 41.09 mM and 78.7 μmol min^?1 mg^?1 protein, respectively. Considering its substrate specificity and other enzymatic characteristics, we believe that this inulinase gene from P. polymyxa ZJ-9 could be transformed into other special bacterial strains to allow inulin conversion to other biochemicals and bioenergy through one-step fermentation.     

超级电容器石墨烯-聚苯胺复合材料的研究进展

超级电容器具有功率密度高、充放电速度快、循环寿命长和维护成本低的特点,在电动车动力电池领域具有潜在的应用前景。超级电容器性能主要由其电极材料所决定。聚苯胺易合成、理论比容量高,而且导电性能优异,作为超级电容器电极材料有很高的应用价值。但是,在长期使用过程中,它的体积容易发生膨胀或收缩,循环寿命差。为了解决这个问题,将聚苯胺与石墨烯复合可以扬长避短,充分利用两者之间的协同效应,赋予复合材料优异电化学电容性能。本文综述了超级电容器用石墨烯-聚苯胺复合材料的制备方法,包括原位聚合法、油水界面合成法、电化学合成法、层层自组装法等;提出了三维网状石墨烯和对石墨烯-聚苯胺复合材料进行改性来提高复合材料的电化学电容性能的思路。