酸量法及碘量法测定氧化葡聚糖的醛基

通过高碘酸钠氧化葡聚糖,制备不同氧化度的葡聚糖,采用酸量法和碘量法测定其醛基含量,但所得结果差异大.结合葡聚糖的氧化机理,以甘油的氧化反应结果作为对照,对借助化学滴定分析的酸量法和碘量法所得数据的差异性进行了分析.结果表明这种差异是由葡聚糖氧化存在的中间反应及其分支结构造成的,当高碘酸钠与葡聚糖的糖单元的物质的量比控制在2以内,操作简单的酸量法所得结果是可靠的.     

气相色谱-质谱法快速测定牛奶中的三聚氰胺和三聚氰酸

建立了气相色谱-质谱法测定牛奶中三聚氰胺和三聚氰酸含量的分析方法。样品经二乙胺-乙腈-水溶液超声提取,离心,滤液用氮气吹干后加入硅烷化衍生试剂衍生,气相色谱-质谱测定,选择离子模式监测,外标法定量。在0.025～2 mg/kg范围内,目标物的峰面积与其质量浓度的线性关系良好(r>0.98);在0.5,1.0和2.5 mg/kg的添加水平,三聚氰胺和三聚氰酸的平均回收率分别为84%～87%和75%～102%,相对标准偏差(RSD)分别为5.7%～11.7%和4.9%～7.8%;三聚氰胺和三聚氰酸的检出限(LOD)分别为0.05 mg/kg和0.10 mg/kg。结果表明:该方法简便、快速、灵敏、准确,适合牛奶中三聚氰胺和三聚氰酸的确证和定量测定。     

纺锤形β-FeOOH纳米结构和α-氧化铁亚微米/微米粒子的合成与转变

使用一种简易的无表面活性剂辅助的水热合成方法,在温度为140 ℃时实现了纺锤形β-FeOOH纳米结构向α-氧化铁亚微米/微米粒子的转变。研究表明,通过实验参数的简单调控,实现了单晶α-氧化铁亚微米粒子与β-FeOOH的纺锤形纳米结构和纳米棒的控制制备。基于实验结果,提出了该过程中的相转变机理。     

YSZ-Al2O3的制备及其负载的单钯密偶催化剂的催化性能

采用胶溶法制备了含YSZ(Y2O3稳定的ZrO2,质量比为1:9)为0,10wt%,15wt%,20wt%,25wt%的YSZ-Al2O3,分别用低温N2吸附-脱附、X射线衍射(XRD)、氨气程序升温脱附(NH3-TPD)技术对它们进行了表征.低温N2吸附结果表明,1000℃焙烧5 h后,钇锆含量为15%的YSZ-Al2O3,有最大的比表面积和孔容,分别达到146 m2·g-1和O.41 mL·g-1,孔径分布集中在9-10 nm.XRD结果表明,添加钇锫的氧化铝以γ相存在,钇锆以固溶体形式存在于氧化铝中.以YSZ-Al2O3材料为载体,采用浸渍法制备了Pd含量为2 g·L-1的单钯密偶催化剂.催化剂活性测试结果表明,添加钇锆能有效地提高催化剂对丙烷的催化活性.当钇锆含量达到15%时,催化剂的起燃温度最低,为275℃.     

Solution‐Based Evolution and Enhanced Methanol Oxidation Activity of Monodisperse Platinum–Copper Nanocubes

Shape‐controlled catalysis : High‐quality Pt–Cu nanocubes with an average size of about 8 nm (see picture, scale bar=20 nm) were synthesized from a high‐temperature organic solution system in the presence of various capping ligands. These cubic Pt–Cu nanocrystals terminated with {100} facets demonstrated a superior catalytic activity towards methanol oxidation compared to similar sized Pt–Cu and Pt nanospheres.

     

Enhanced Electrogenerated Chemiluminescence of Tris(2,2′‐bipyridyl) Ruthenium(II)/tripropylamine in the Presence of Pyridine and Its Analogues

In the present work, we conducted an investigation on the electrochemical and ECL behavior of Ru(bpy) /TPrA system in the presence of pyridine and its analogues on platinum and gold electrode. Results showed that pyridine and its analogues enhanced Ru(bpy) /TPrA ECL signal and exhibited different enhancement effects on different electrodes. On platinum electrode, the maximum enhancement factor of about 5 was obtained. On gold electrode, a low‐oxidation‐potential (LOP) ECL signal occurred and increased.     

Three New Alkaloids from the Leaves of Uncaria rhynchophylla

Three new alkaloids, 2′‐O‐β‐D ‐glucopyranosyl‐11‐hydroxyvincoside lactam ( 1 ), 22‐O‐demethyl‐22‐O‐β‐D ‐glucopyranosylisocorynoxeine ( 2 ), and (4S)‐corynoxeine N‐oxide ( 3 ) were isolated from the leaves of Uncaria rhynchophylla, together with four known tetracyclic oxindole or indole alkaloids, isocorynoxeine N‐oxide ( 4 ), rhynchophylline N‐oxide ( 5 ), isorhynchophylline N‐oxide ( 6 ), and dihydrocorynantheine ( 7 ), and an indole alkaloid glycoside, strictosidine ( 8 ). The structures of 1 – 3 were elucidated by spectroscopic methods including UV, IR, ESI‐TOF‐MS, 1D‐ and 2D‐NMR, as well as CD experiments. The activity assay showed that 8 (IC₅₀=8.3 μM ) exhibited potent inhibitory activity on lipopolysaccharide(LPS)‐induced nitrogen monoxide (NO) release in N9 microglia cells. However, only weak inhibitory activities were observed for 1 – 7 (IC₅₀>100 μM for 1 – 6 or >30 μM for 7 ).     

超临界CO2微乳/反胶束体系热力学行为与应用*

超临界微乳/反胶束体系极大地拓展了超临界流体的溶剂特性,是超临界流体技术研究的热点课题。选择合适的表面活性剂,通过调控操作条件,可以方便地控制其增溶特性,作为一种新兴绿色溶剂,在化学反应、材料制备、萃取分离等领域都有潜在的应用前景。本文阐述了超临界CO₂微乳/反胶束系统的基本概念,总结和归纳了关于热力学性质、表面活性剂选择、相行为、水力学尺寸计算、聚团颗粒间相互作用力等理论研究成果。在此基础上,还就该领域的一些应用进行了分析讨论。     

Precipitation and recrystallization of uniform CuCl particles formed by aggregation of nanosize precursors

Uniform, spherical CuCl particles were obtained by mixing aqueous solutions of CuCl ₂ and ascorbic acid in the presence of polyvinylpyrrolidone (PVP) as dispersing agent. The size and the uniformity of the resulting particles depended on the volume ratio of the reactant solutions, their concentrations, the distribution of the stabilizers, and the mixing method. The single jet precipitation yielded large spheres of broad size distributions, while the particles obtained by the double jet technique were rather uniform in size. The final colloidal CuCl particles were formed by the aggregation of nanocrystals, initially generated in the system. Depending on the pH of the reaction mixture, these particles slowly change to large CuCl crystals on aging in the mother liquor.     

Morphology Control over the Organic Nanoparticles of 1,3-Diphenyl-5-（9-anthryl）-2-pyrazoline

The organic nanoparticles of a blue-light-emitting molecule, 1,3-diphenyl-5-(9-anthryl)-2-pyrazuline, were prepared by reprecipitation method using acetonitrile as the solvent for the molecular precursor. Three morphologies, spherical, doughnut-shaped and cubic, could be observed on the silicon substrate forthe nanoparfides by the volume-controlled addition of acetonitrile. The evolution of particle morphology as a function of acetonitrile addition was attributed to the variation of the growth habits of the particles in the different environment. The nanoparticles exhibit the novel photoluminescence spectra as compared to those of monomer and the bulk crystals.