系列单取代烷氧基-2-羟丙基-β-环糊精的合成与表征

以环氧氯丙烷和脂肪醇为原料, 通过相转移催化法合成了乙基、正丙基、正丁基和正戊基缩水甘油醚(1～4), 并利用所合成的缩水甘油醚和β-环糊精为原料, 分别在弱碱水溶液(1.5%)和强碱水溶液(30%)中制备并用硅胶柱分离出单2位取代的乙氧基、丙氧基、丁氧基和戊氧基-2-羟丙基-β-环糊精(1a～4a)和单6位取代的丙氧基、丁氧基和戊氧基-2-羟丙基-β-环糊精(2b～4b), 利用薄层色谱、红外光谱、差热扫描量热分析、质谱和核磁共振等手段对所合成的产品进行了表征.     

A New Amperometric Biosensor Based on HRP/Nano-Au/L-Cysteine/Poly（o-Aminobenzoic acid）-Membrane-Modified Platinum Electrode for the Determination of Hydrogen Peroxide

The third generation amperometric biosensor for the determination of hydrogen peroxide （H2O2） has been described. For the fabrication of biosensor, o-aminobenzoic acid （oABA） was first electropolymerized on the surface of platinum （Pt） electrode as an electrostatic repulsion layer to reject interferences. Horseradish peroxidase （HRP） absorbed by nano-scaled particulate gold （nano-Au） was immobilized on the electrode modified with polymerized o-aminobenzoic acid （poABA） with L-cysteine as a linker to prepare a biosensor for the detection of H2O2. Amperometric detection of H2O2 was realized at a potential of ＋20 mV versus SCE. The resulting biosensor exhibited fast response, excellent reproducibility and sensibility, expanded linear range and low interferences. Temperature and pH dependence and stability of the sensor were investigated. The optimal sensor gave a linear response in the range of 2.99×10^-6 to 3.55×10^-3 mol·L^-1 to H2O2 with a sensibility of 0.0177 A·L^-1·mol^-1 and a detection limit （S/N = 3） of 4.3×10^-7 mol·L^-1. The biosensor demonstrated a 95% response within less than 10 s.     

6-甲氧基-2-丙酰基萘在醇溶剂中的溴化反应

室温下，6－甲氧基－2－丙酰基萘和1，3－二溴－5，5－二甲基海因的溴化反应在醇溶剂中，反应速度快、转化率高，生成5－溴－6－甲氧基－2－丙酰基萘的收率高（98．59％）。     

Electrochemical Characteristics of Mg0.9Ti0.1-xZrxNi （x=0.02, 0.04, 0.06） Alloys

Mg-based hydrogen storage alloys Mg0.9Ti0.1-xZrxNi (x=0.02, 0.04, 0.06) were successfully prepared by means of mechanical alloying (MA). The effects of Zr addition on the discharge capacity and the cycle performance of the Mg-based electrodes were also studied. It was found that the discharge capacities were improved with addition of a small amount of Zr and the cycle performances of the alloy were stabilized with the addition of Ti. The effects of surface modification or coating on the properties of Mg0.9Ti0.06Zr0.04Ni were also studied. The results indicated that coating with graphite improved both the discharge capacity and cycle life of the amorphous Mg0.9Ti0.06Zr0.04Ni electrode.     

Highly Selective Salicylate Membrane Electrode Based on N,N＇- （Aminoethyl）ethylenediamide Bis（2-salicylideneimine） Binuclear Copper（Ⅱ） Complex as Neutral Carrier

A new ion selective electrode for salicylate based on N,N＇-（aminoethyl）ethylenediamide bis（2-salicylideneimine） binuclear copper（Ⅱ） complex [Cu（Ⅱ）2-AEBS] as an ionophore was developed. The electrode has a linear range from 1.0 × 10^-1 to 5.0 ×10^-7 mol·L^- 1 with a near-Nemstian slope of （ - 55 ±1 ） mV/decade and a detection limit of 2.0 × 10-7 mol·L^-1 in phosphorate buffer solution of pH 5.0 at 25 ℃. It shows good selectivity for Sal^- and displays anti-Hofmeister selectivity sequence： Sal^-〉SCN^-〉 ClO4^- 〉I^-〉 NO2^- 〉Br^-〉 NO3^- 〉Cl^-〉 SO3^2- 〉 SO4^2- The proposed sensor based on binuclear copper（Ⅱ）complex has a fast response time of 5-10 s and can be used for at least 2 months without any major deviation. The response mechanism is discussed in view of the alternating current （AC） impedance technique and the UV-vis spectroscopy technique. The effect of the electrode membrane compositions and the experimental conditions were studied. The electrode has been successfully used for the determination of salicylate ion in drug pharmaceutical preparations.     

2-巯基噻唑[5，4-d]并嘧啶类化合物及其衍生物的合成

由邻硝基氯代嘧啶（3）为原料料，与多硫化钠和二硫化碳共煮，经一步反应 获得了2-巯基噻唑[5，4-d]并嘧啶（4）。由4出发，合成了一系列2位取代的衍生 物5，4和5的结构均通过了~1H NMR及元素分析确让。并对少数化合物的生物活性进 行了测试。     

STUDIES ON IMMOBILIZED GLUCOSE OXIDASE BY DIETHYLAMINOETHYL CELLULOSE COMPLEXES

The properties of immobilized glucose oxidase (GOD) by the complexes of diethylaminoethyl cellulose(DEAEC) with different polymers, such as polymethylacrylic acid (PMAA), polyacrylic acid (PAA), polystyrene sulfonic acid (PSSA), polyvinylaleohol (PVA), polyethylene oxide (PEO) and styrene-maleic acid copolymer (PSMA) were investigated. The activity of immobilized GOD was obviously influenced by the component of the DEAEC complexes. The relative activity of the immobilized GOD reached to maximum and over 90% of the native GOD. when the DEAEC-PMAA DEAEC-PAA complexes were used as a carrier with the molar ratio of DEAEC and polyacid of about one. Michaelis constants (Km) of the immobilized enzymes of DEAEC-GOD-PMAA and DEAEC-GOD-PAA were determined to be 1.25 and 1.00, respectively. Moreover, the immobilized GOD has a good storage stability and cyclic life.     

Thermochemical Properties and Decomposition Kinetics of Ammonium Magnesium Phosphate Monohydrate

Ammonium magnesium phosphate monohydrate NH4MgPO4·H2O was prepared via solid state reaction at room temperature and characterized by XRD, FT-IR and SEM. Thermochemical study was performed by an isoperibol solution calorimeter, non-isothermal measurement was used in a multivariate non-linear regression analysis to determine the kinetic reaction parameters. The results show that the molar enthalpy of reaction above is （28.795 ± 0.182） kJ/mol （298.15 K）, and the standard molar enthalpy of formation of the title complex is （-2185.43 ± 13.80） kJ/mol （298.15 K）. Kinetics analysis shows that the second decomposition of NH4MgPO4·H2O acts as a double-step reaction： an nth-order reaction （Fn） with n=4.28, E1=147.35 kJ/mol, A1=3.63×10^13 s^-1 is followed by a second-order reaction （F2） with E2=212.71 kJ/mol, A2= 1.82 × 10^18 s^-1.     

基于碘乙酸功能化树枝状聚合物的硫巯化肽段选择性富集新方法

蛋白质的硫巯化是一种重要的氧化翻译后修饰，在细胞衰老、内质网应激、血管舒张、细胞凋亡等过程中扮演重要角色。利用蛋白质组学技术表征硫巯化修饰具有十分重要的意义。该文发展了一种基于碘乙酸功能化的聚酰胺-胺树枝状聚合物（PAMAM-INS），并结合滤膜辅助的样品预处理技术用于硫巯化肽段的富集（简称FADE策略），利用FADE策略能从100倍质量干扰的牛血清白蛋白酶解产物中选择性地富集出硫巯化标准肽段。将细胞培养稳定同位素标记技术引入到FADE策略中，并将其应用于不同浓度梯度硫氢化钠刺激的SHSY5Y细胞硫巯化蛋白质组分析，共鉴定到163条硫巯化肽段。生物信息学的结果表明，硫巯化修饰可能在中枢神经系统中扮演着重要角色。     

Cd2Ge7O16中Tb的长余辉发光特性

本文研究了Cd₂Ge₇O₁₆∶Tb³⁺材料的发光及其长余辉性质。指出Tb³⁺的发光是该离子的 ⁵D₃- ⁷D_J、 ⁵D₄- ⁷D_J两种跃迁产生的；随着掺杂浓度的增加 ⁵D₄- ⁷D_J跃迁增强，发光颜色由蓝变绿。并把该材料的长余辉性质归结为基质结构中有电子陷阱和空穴陷阱。提出余辉机理模型。