碳水化合物衍生的手性配体——25含碳水化合物单元的膦配体在钯催化的Heck反应中的应用

评价了一种碳水化合物衍生的具有较大立体位阻及较三苯基膦更富电子的膦配体(甲基3-脱氧-3-二苯膦基-4,6-氧-苯次甲基-α-D-吡喃阿卓糖苷,3-MBPA)在Pd催化的Heck反应中的性能.发现在N,N-二甲基乙酰胺溶刺中K2CO3是该催化体系较适合的碱;在该配体的支持下催化剂中钯的用量可低至0.5 mo1%;可催化苯乙烯与带给电子基团的溴代芳烃及带吸电子基团的氯代芳烃发生反应,高产率地生成相应的偶联产物;反应区域选择性表明,Pd(OAc)2/3-MBPA体系在催化苯乙烯与卤代芳烃的Heck反心中并存阳离子催化途径,说明3-MBPA中的氧原了可能也参与配位;同时发现,加入助配体四丁基溴化胺(TBAB)后,可能是Br-参与配位有利于增加中性催化途径的机会而提高了反应区域选择性.     

Effect of final heating temperature on crystallization of isotactic polypropylene nucleated with an aryl amide derivative as <Emphasis Type="Italic">β</Emphasis>-form nucleating agent

An aryl dicarboxylic acid amide compound TMB-5 is an efficientβ-form nucleating agent for isotactic polypropylene(iPP).Because of the solubility of TMB-5,superstructure and morphology of iPP crystals changed with melting conditions.Effects of final heating temperature(T_f)on heterogeneous nucleation of iPP/TMB-5 were investigated.It was discovered that the crystallization temperature increased with decreasing T_f value.The optical microscopic images indicated that when TMB-5 partially dissolved in iPP melt,the remaining(non-dissolved)TMB-5 facilitated the recrystallization of dissolved nucleating agent from the melt,which promoted crystallization.Complete solubility of nucleating agent caused the decreasing efficiency.TMB-5 recrystallized in the form of tiny needles,whose aggregates induced dendritic iPP crystals.     

Production of Recombinant Porcine Interferon alpha Using PHB–Intein-Mediated Protein Purification Strategy

Interferons (IFNs) are involved in the pathogenesis and recovery of viral and other infectious diseases. Recombinant IFNs have been used as anti-infectious agents exhibiting a broad range of antiviral and immunomodulatory properties in both human and domestic animals. In this report, we describe a highly efficient and economical approach to purify porcine IFN alpha (PoIFNα) using polyhydroxybutyrate (PHB) as the affinity carrier and intein for self-cleaving removal of the affinity tag. Additionally, the conditions of protein expression and purification have been optimized. Our results suggested that culture medium containing 1.62% (w/v) of sodium lactate dramatically increases the accumulation of PHB binding protein in Escherichia coli cells. High yields of recombinant PoIFNα (30–35 mg/L, 97% purity by high-performance liquid chromatography) were obtained using intein-mediated self-cleaving conditions using a cleavage-inducing buffer with a pH of 6.5 at 20 °C for 24–36 h. The antiviral activity of the recovered recombinant PoIFNα was up to 1.4 × 10⁶ IU/mg of protein ascertained using recombinant human IFNα1 as a standard. This report also demonstrates that large-scale production of intein-mediated purification of highly pure and active recombinant PoIFNα is feasible for the purposes of experimental studies, veterinary clinic therapeutics, and swine infectious disease control.     

Identification of [PtCl2(phen)] binding modes in amyloid-β peptide and the mechanism of aggregation inhibition

Platinum phenanthroline complexes inhibit amyloid-β (Aβ) aggregation and reduce Aβ-caused neurotoxicity [Proc. Natl. Acad. Sci., 2008, 105, 6813-6818]. In this study, we investigated the interactions of Aβ(1-16) with [PtCl(2)(phen)] (phen=1,10-phenanthroline) using HPLC, ESI-MS, and NMR spectroscopy , and characterized the identity of products using tandem mass spectrometry. Results indicated that the phenanthroline ligand could induce noncovalent interactions between Aβ peptide and platinum complexes, leading to rapid Aβ platination. Multiple products were generated in the reaction, in which His6/His14 chelation was preferentially formed. Coordination of Asp7, His13, and Lys16 was also detected in other products. The majority of products were monoplatinated adducts with binding of the {Pt(phen)} scaffold, which impeded intermolecular interactions between Aβ peptides. Moreover, noncovalent interactions were confirmed by the interaction between Aβ peptide and [Pt(phen)(2)]Cl(2). The synergistic roles of the phen ligand and platinum(II) atom in the inhibition of Aβ aggregation are discussed.     

HPLC-MS/MS法联合分析环境水体中喹诺酮类抗生素和雌激素

建立了环境水体中15种喹诺酮类抗生素和6种雌激素的HPLC-MS/MS分析方法.该方法统一了两类物质的前处理过程,运用固相萃取技术进行富集及净化,有效降低了基质的干扰.质谱采用SRM监测模式,喹诺酮采用正离子扫描模式,雌激素采用负离子扫描模式.目标化合物在水体中的回收率范围为62.0％～108.3％,RSD在1.1％ ...     

辊速辊温对高密度聚乙烯拉伸微孔膜及其片晶结构的影响

采用熔融挤出片材—退火—冷拉伸—热拉伸—热定形的方法来制备高密度聚乙烯(HDPE)微孔膜,利用FTIR、SEM和DSC等测试方法来研究辊速辊温对HDPE拉伸微孔膜及其片晶结构的影响.研究结果表明,所选树脂的分子量、分子量分布以及弛豫时间能够满足现有加工条件,形成片晶取向度较高的预制膜;在相同辊温下,随辊速增加,退火前预...     

微波辐射法制备水溶性CdTe/ZnS量子点及其与司帕沙星的作用

以巯基乙酸为稳定剂,通过微波加热在水溶液中制备了CdTe/znS量子点.研究了pH值、反应时间、反应温度和cdTe/s<'2->浓度比等合成条件对cdTe量子点荧光光谱的影响.以CdTe/ZnS量子点为探针,探讨了喹诺酮类抗生素司帕沙星与量子点的荧光猝灭作用,结果表明,在最佳实验条件下,其线性范围为0.05～3.00μg/mL,线性相关系数为0.9954,检出限为0.01μg/mL,可将CdTe/ZnS量子点荧光探针用于司帕沙星的测定.