Ham理论的验证及其应用

利用直拉硅单晶中氧化物沉淀的生长，选择两步热处理制度，验证了Ｈａｍ有关扩散控制沉淀生长理论。并尝试应用Ｈａｍ理论对氧化物沉淀的形核进行处理。 关键词：     

钙对铝水解聚合反应及聚合铝物化特性的影响

The polyaluminum chloride containing Ca was prepared by adding Ca before and after the aluminium polymerization, respectively. The effects of Ca on the hydrolysis and polymerization of aluminum, the characteristic of aluminum species, the ζ potential and viscosity of PAC were also studied. The experimental results show that the introduction of Ca retards the formation of Al precipitates during the hydrolysis and polymerization of aluminum and increases the contents of Al_m and Al₁₃ in PAC. Aluminum species can complex with Ca to form heteronuclear hydroxo complexes, which decreases the chemical shifts of Al_m and Al₁₃ in NMR. The ζ potential and the viscosity of PAC increase with the rise of Ca/Al molar ratio. Comparing with adding Ca after the aluminium polymerization, there are much more Al-Ca heteronuclear hydroxo complexes formed by adding Ca before the polymerization, which leads to a more obvious influence of Ca/Al molar ratio on the ζ potential and the viscosity of PAC.     

3-O-甲基槲皮素的合成

以芦丁为原料经苄基化、酸水解、选择性甲基化和氢化脱苄四步反应,合成了3-O-甲基槲皮素,总收率为76%.利用1H NMR和MS对中间体及产物的结构进行了确证.该发现有望为3-取代槲皮素衍生物的合成提供一条捷径.     

丙三醇水溶液玻璃结构松弛现象学研究

为了考察水含量对丙三醇水溶液玻璃体结构松弛行为的影响，利用差示扫描量热法(DSC)测量了五种高浓度丙三醇水溶液的玻璃化转变温度和玻璃化转变区域的比热容，利用TNM模型进行了结构松弛的现象学分析. 松弛时间的分析结果表明，水溶液玻璃中水含量越高，则松弛过程越快. TNM模型的计算结果表明，随着水含量的增加，玻璃体系的结构松弛活化能和非指数参数都有逐渐降低的趋势，而非线性参数和指前因子逐渐增加.     

用DSC测量葡萄糖溶液部分玻璃化转变温度的新方法

用差示扫描量热仪, 采用经过退火处理的连续扫描法, 以不同浓度(20%、45%)的葡萄糖溶液为研究对象, 研究了退火温度对Tgf(部分结晶的玻璃化转变温度)的影响, 给出了确定Tg′(部分玻璃化转变温度)的新方法. 研究发现, 不同退火温度下的Tgf不同. 在−50 ℃以上退火, Tgf随着退火温度的增大而减小; 在−50 ℃以下退火, Tgf随着退火温度的增大而增大, 都有很好的线性关系. 不同浓度的溶液具有相似的规律. 提出从Tgf确定Tg′的方法: Tgf在−50 ℃上下随退火温度变化线的交点所对应的部分结晶玻璃化转变温度即为Tg′. 使用该方法测得葡萄糖的Tg′为−55 ℃.     

氨基酸锑(Ⅲ)双核配合物的固相合成与表征

采用室温固相反应法合成了甘氨酸锑和苯丙氨酸锑双核配合物 ,用元素分析、远红外光谱、热重差热分析及X射线粉末衍射进行了表征 .两种配合物Sb2 L5X·2 5H2 O(L =gly ,phe;X =Cl或I)的晶体结构均属于单斜晶系 ,甘氨酸锑配合物的晶胞参数为 :a =0 6 5 2 6nm ,b =1.2 2 2 7nm ,c=1.3877nm ,β=97.88°,V =1.0 96 8nm3 ,苯丙氨酸锑配合物的晶胞参数为 :a =1.0 6 17nm ,b =0 .7839nm ,c =1.5 72 5nm ,β =92 .32°,V =1.30 77nm3 .远红外光谱表明O ,N ,Cl或I原子参与配位     

Determination of Pharmacokinetics of Tanshinone II A in Mouse Plasma and Brain by High Performance Liquid Chromatography

High performance liquid chromatography (HPLC) method was developed to measure the concentration of tanshinone IIA (Ts IIA) in mouse plasma and brain. The method was applied to preliminary study on pharmacokinetics of Ts IIA in mouse plasma and brain. After an administration of 8.0 mg kg⁻¹ of Ts IIA by an intravenous injection, plasma and brain samples were collected and extracted by liquid-liquid extraction with ethyl acetate and determined by HPLC. This method has a linear range from 0.05 to 7.12 mg l⁻¹ with correlation coefficients of 0.9984 in plasma and a linear range from 0.022 to 2.37 mg l⁻¹ with correlation coefficients of 0.9988 in brain. The limits of quantitation in plasma and brain were 0.050 and 0.022 mg l⁻¹, respectively, and the limits of detection were 0.026 and 0.017 mg l⁻¹, respectively. The intra-day and inter-day precisions were less than 10.3%. The developed method was selective, accurate, and sensitive and can be applied to determine the concentration of Ts IIA in mouse plasma and brain quantitatively after intravenous administration of Ts IIA. It was suitable for the pharmacokinetic study of Ts IIA. The plasma concentration-time curve was fitted as three-compartment model. The peak concentration of Ts IIA in mouse plasma was 1.58 mg l⁻¹, and the value of the areas under the plasma concentration-time curve (AUC 0-t) was 68.18 mg l⁻¹ min⁻¹. The concentration of Ts IIA in mouse brain achieved the peak value of 0.17 mg l⁻¹ 5 min after mainlined, and Ts IIA could be still detected in brain 480 min after mainlined. The results indicated that Ts IIA readily penetrated the blood-brain barrier and could stay in the brain for a long time.     

基于分子印迹膜的检测牛奶中琥珀酸氯霉素残留传感方法的研究

采用光聚合法在一次性丝网印刷电极上制备琥珀酸氯霉素分子印迹膜,然后将丝网印刷电极通过电极插口与电化学分析装置相连接,组装成检测琥珀酸氯霉素残留的电化学传感仪.使用与传感装置相连接的记录仪记录响应的结果.采用本传感仪建立了检测氯霉素的标准曲线并测试了实际牛奶样品中氯霉素含量.电镜学观察表明,与非印迹膜相比,在印迹膜表面形成大量直径约为100 nm的印迹微孔.本传感仪装置检测琥珀酸氯霉素具有很高的灵敏度和特异性,检出限为2×10-9 mol/L,检测线性范围为1×10-8～1.2×10-5 mol/L,基于牛奶样品的检测回收率介于93.5%～95.5%之间.     

硫杂蒽酮镍（II）配合物与DNA的作用研究

合成了O-（硫杂蒽酮-[2]-基）-氧乙酸镍（II）配合物。通过元素分析,IR, DTA-TG谱对其结构进行了表征。研究表明：配体羧羰基脱质子后与镍离子配位,配合物中含有一定量的配位水。同时以紫外可见光谱、荧光光谱、园二色谱,电化学方法和凝胶电泳方法研究了该配合物与DNA的作用。结果表明,该配合物能在生理条件下比配体和金属离子更有效地切割质粒DNA,自由基捕捉剂的加入不影响配合物的切割活性。该配合物使DNA溶液的紫外吸收强度和园二色吸收强度降低,DNA的存在可使该配合物的氧化还原活性降低。与溴化乙锭和DNA的竞争反应说明,该配合物主要以嵌入方式与DNA结合。