Influence of thermal and thermo-mechanical treatment

Two lipids with similar melting ranges but of different composition were analyzed using differential scanning calorimetry and X-ray diffraction. The lipids were processed via extrusion or were tempered at different temperatures; they were analyzed directly after extrusion and after storage at 40°C. Precirol ATO 5® showed high sensitivity to storage time and varied temperature exposure. Extrusion showed only marginal influences on the solid state. Melting peaks were narrower and shifted to higher temperatures in comparison to the untreated powder. Dynasan 114® was more robust, changes in the solid state could only be shown for samples treated above the melting range. Thus, Dynasan 114® is more appropriate for solid lipid extrusion of pharmaceutical products.     

Calorimetric approach to tetronic/water interactions

Tetronic^®comprises X-shaped copolymers formed by four poly(propylene oxide) (PPO) andpoly(ethylene oxide) (PEO) block chains bonded to an ethylene diamine centralgroup. Micellization behaviour of three representative Tetronics (T304, T904and T1307) was characterized to gain an insight into the interactions betweenthe copolymer unimers and the state of water in their solutions. The enthalpyof demicellization, recorded at 37°C in an isoperibol microcalorimeter,indicated that the process was in all cases exothermic and the enthalpy rankedin the order T1307≥T904>>T304. Micellization is entropy-driven owing tohydrophobic interactions between the PPO chains.DSC analysisshowed that the crystallization and melting peaks of the free water remainingin T304 and T904 solutions were progressively shifted toward lower temperaturesas the surfactant proportion increased, owing to a colligative effect. Boundwater corresponded to 3 water molecules per EO repeating unit. In the caseof T1307, which has longer PEO chains, a splitting of the melting peak wasobserved, one peak appearing around 0°C due to free water and anotherat –15°C due to interfacial water. As T1307 proportion raised, theenthalpy of the former decreased, whilst the enthalpy of the latter increased.In 40% T1307 solutions, interfacial water overcame the proportion of freewater; there being 1 interfacial and 3 bound water molecules per EO repeatingunit. Gaussian deconvolution of FTIR spectra also enabled to characterizethe evolution of free water as a function of Tetronic proportion. The dependenceof micellization and water interaction behaviour on Tetronics structure shouldbe taken into account to use these copolymers as drug solubilizers and micellarcarriers.     

8-羟基喹啉-5-磺酸纤维微柱分离富集电感耦合等离子体原子发射光谱法同时测定多种痕量元素

本文合成了8-羟基喹啉-5-磺酸纤维滤纸片,以此做为微柱填充物同时富集了10种痕量元素,并分离了样品中的高盐组分.本方法可使痕量组分的分离与富集同步进行,因而特别适用于原子光谱测定前样品的预处理.     

DNA intercalating studies of [Ru(bpy)<Subscript>2</Subscript>HPIP]<Superscript>2+</Superscript> with intramolecular hydrogen bond ligand based on introduction of copper ion

The effects of copper ion on the interaction of [Ru(bpy)₂HPIP]²⁺(bpy = 2,2′-bipyridine, HPIP = 2-(2-hydroxyphenyl) imidazo [4,5-f] [1, 10] phenanthroline) with DNA have been investigated by electronic absorption spectroscopy and fluorescence spectroscopy. HPIP ligand of the complex with an intramolecular hydrogen bond can bind Cu²⁺ in the absence of DNA, as revealed by the absorbance and fluorescence decrease for [Ru(bpy)₂HPIP]²⁺. The resultant heterometallic complex binds to DNA via intercalation of HPIP into the DNA base pairs and its DNA-binding ability is stronger than [Ru(bpy)₂HPIP]²⁺ itself. The DNA bound [Ru(bpy)₂HPIP]²⁺ cannot bind Cu²⁺ at low Cu²⁺ concentration and the intramolecular hydrogen bond in HPIP is located inside the DNA helix. While the Cu²⁺ concentration is relative high, Cu²⁺ can quench the fluorescence of DNA bound [Ru(bpy)₂HPIP]²⁺. The quenching reason is proposed.     

Cl/Ag体系研究 Ⅱ.Cl吸附引起的表面结构变化

运用LEED,UPS和HREELS等表面技术研究了氯吸附至(c)阶段的Ag(111)表面结构.结果表明,表面上有三维的AgCl(111)生成,其生长按修正的Stranski-Krastanov模式进行.伴随着AgCI(111)生长的同时,表面上产生缺陷.这种缺陷只有在氯吸附至(c)阶段时表面上形成三维AgCI的过程中才能产生,它一旦在表面上形成后,表面上氯的存在与否对其不产生影响.本文提出了一个(c)阶段时的Cl/Ag(111)体系的结构模型.     

氨基羧酸纤维分离富集-电感耦合等离子体原子发射光谱法测定多种痕量稀土元素

本文制备了氨基羧酸纤维滤纸片作为柱填充物，成功地分离和富集了地化样品中的多种稀土元素。富集后的稀土元素采用电感耦合等离子体原子发射光谱法测定，回收率为90％～109％。本文还对基体干扰及其消除进行了研究。     

氧极谱催化波法测定二苯胺

本文报道一种极谱测定二苯胺的新方法,它是基于二苯胺引起的氧极谱催化波.这个氧极谱催化波是由于二苯胺催化了电生超氧离子O_2~(-)的歧化反应产生的.本方法简单方便,有良好选择性.应用本方法测定了化工原料二苯胺的含量,结果令人满意.     

Structural Study of Silica Xerogel Composites Containing Pd Aggregates

Composites containing Pd aggregates dispersed in amorphous silica are of interest from both a fundamental and applied point of view because of their attractive catalytic properties. The silica powders added with palladium, prepared by the sol-gel method, were studied using X-ray diffraction, and IR- and UV-Vis-spectrophotometry. Silica xerogel samples were prepared using a ethanol/H₂O/TEOS molar ratio of 4:11.6:1 and loaded with sodium tetrachloropalladate. The silica xerogel microstructure of the powders was studied as a function of annealing temperature. Attention was paid to the evolution of the glass matrix as well as the palladium aggregates in the SiO₂ matrix. We found in our samples partial crystallization of the glass matrix in form of quartz and cristobalite phases with palladium oxide and metallic palladium phase at 1000^∘C. The Rietveld refinement method was used in order to determine the percentage of the phase contents.     

环境样品中痕量邻苯二甲酸酯的分离与测定

本文研究了以小粒径（１０－４０μ）硅胶柱色谱分离富集、反相高效相色谱分析测定大气颗粒物、土主植物样品中痕量邻苯二甲酸酯的方法，方法操作简单，回收率高，空白值低，利用该方法分析了部分环境样品中邻苯二甲酯酯含量。     

Synthesis and in vivo study of metallofullerene based MRI contrast agent

Gd@C₈₂(OH)₄₀ has been developed as a new generation of MRI contrast agent. But recently, it was found that Gd@C₈₂(OH) _x with a larger number of OH (x>36) would lead to cage break and hence, release of highly toxic Gd ions. We synthesized the more stable Gd@C₈₂(OH) _x with less OH-number, Gd@C₈₂(OH)₁₆, and studied its proton relaxivity and MRI images. The results indicate that Gd@C₈₂(OH)₁₆ also gives high proton relaxivity, even higher than that of (NMG)₂-Gd-DTPA. The bio-distribution indicated that Gd@C₈₂(OH)₁₆ tends to be entrapped in the liver and kidney and remained in tissue for about 2 hours. The results suggest that the more stable metallofullerene derivative Gd@C₈₂(OH)₁₆ can be the potential candidate of the new MRI contrast agent.