光度分析法在药物分析中的研究与应用

综述了国内近年来光度分析法在药物分析中的研究与应用情况.就分光光度法、荧光光度法、化学发光法3种重要的分析方法,从反应条件、线性范围、灵敏度等方面介绍了光度分析法对不同反应体系的研究现状,展望了光度分析法在药物分析中的发展方向.     

β-环糊精与莨菪类药物包结反应的热力学研究

研究了β-环糊精与四种莨菪类药物的包结反应.微量量热法研究表明,反应中均生成1:1包结配合物,并测出各反应的热力学参数K,△G°,△H°与△S°.~1H NMR谱表明,药物分子被包结在β-环糊精分子疏水性空穴内.初步讨论了反应作用力的性质、客体分子的手征性及其分子空间环境对包结反应的影响.     

用相关判别法研究—水合草酸钙脱水过程

目前,用热分析技术研究固体热分解反应动力学成了一个十分活跃的研究领域.但是,不同的研究者所公布的动力学参数往往有很大的差别,其原因固然是多方面的,最主要的是没有一种可靠的方法判别正确的分解反应机理.过去对反应机理的判别较多地是采用热重分析的相关系数一步判别法,由于热重分析的相关系数大都比较接近,因此仅靠这种单一的方法,很难作出准确判断.如果将等温热重分析的相关系数判别法、非等温与等温热重分析的动力学参数判别法和反应速率常数的对比判别法三者结合起来,则可以大大地提高判断的准确度.本文以一水合草酸钙为例,表明这种相关判别法的适用性.     

热动力学时间变量法——简单级数化学反应

在热动力学理论基础上提出了一种新的热动力学研究法--时间变量法.该法无须将反应进行到底,只需知道一张热谱图上的3个时间点t,t时刻峰高△和t前峰面积a,就可用计算机数值方法求算反应的速率常数.应用该法研究了一级反应、等浓度二级反应、不等浓度二级反应、三级反应和1.5级反应的热动力学.     

多种方法分析与评价乙酸乙酯合成实验中产物之纯度

采用气相色谱内标法、面积归一化法及NMR内标法3种方法对乙酸乙酯合成反应中的产物进行纯度分析.GC内标法可抵消由于操作条件的波动而带来的误差,只需内标物与待测组分在同样条件下出峰且分离度较好,定量精度高,测出的乙酸乙酯纯度最低;应用NMR内标法可同步完成纯度分析和结构鉴定,且无需引入校正因子,操作简便.     

硫酸-甲醛反应在药物荧光分析中的应用

硫酸-甲醛反应(即Marquis反应)是药物定性鉴定的一种颜色反应,有300余种药物能与硫酸甲醛试剂反应产生不同的颜色,由此可进行药物的定性分析。本文研究了硫酸甲醛反应在药物荧光定量分析中的应用,在初步研究的13种药物中,有11种药物得到增强的荧光信号。此法可提高药物荧光测定的灵敏度和选择性,在药物分析方面具有广阔的应用前景。     

二氧化硅负载氧化锌催化剂的溶胶-凝胶和浸渍法制备及对仲丁醇分解反应的催化性能

分别采用溶胶-凝胶法和浸渍法制备了ZnO-SiO₂催化剂和ZnO/SiO₂催化剂并进行了表征, 以仲丁醇脱氢为探针反应, 研究了不同制备方法对催化剂表面ZnO物种存在状态及其催化性能的影响. 结果表明, 2种方法均可制备高分散的负载型ZnO催化剂. 在ZnO-SiO₂和ZnO/SiO₂催化剂上, 仲丁醇分别以脱水和脱氢反应为主. 经过分析, 催化剂上ZnO物种的存在状态是影响产物选择性的关键因素, 而2种催化剂表面的粒径、 比表面积和表面酸碱性不是影响该反应选择性的根本原因.     

邻苯三酚自氧化反应的动力学研究

利用单扫示波极谱法(并辅以紫外-可见光谱法)研究了邻苯三酚在pH7.20～9.10的Tris－HCl缓冲体系中自氧化反应的动力学.结果表明, 在过量溶解O₂存在时, 反应对邻苯三酚为一级.在一定pH范围内, 准一级反应表现速率常数K_app随pH值的增加而增加, 说明H₂PYR-比H₃PYR对溶解O₂具有更高的反应活性.探讨了邻苯三酚自氧化生成半醒自由基和活性氧的反应机理, 用速率方程解释了实验现象.并为酶活力测定和药物抗氧活性研究提供了一种新方法.     

有机药物分析与吸附伏安法

本文评述了有机药物分析的重要作用和意义，有机药物的一般性质，吸附伏安法的特点及其应用。     

降解PET聚酯瓶实验条件的研究——综合研究型实验设计

为了从废PET聚酯瓶中回收对苯二甲酸(TPA),分别对比研究了酸性水解法、肼解法和醇碱联合法降解PET聚酯瓶的反应收率及环境友好性、经济性等.通过正交实验,探索了醇碱联合解聚法的最佳反应条件.采用红外光谱对回收的对苯二甲酸进行了表征,结合量子化学计算对振动光谱和分子间氢键进行了研究.     

Determination of Quality Properties of Soy Sauce by Support Vector Regression Coupled with SW-NIR Spectroscopy

The modern near-infrared(NIR) spectroscopy analysis is a simple, efficient and nondestructive technique, which has been used in chemical analysis in diverse fields. Shortwave NIR spectroscopy is also a rapid, flexible, and cost-effective method to control product quality in food industry. The method of support vector regression coupled with shortwave NIR spectroscopy was explored for the nondestructive quantitative analysis of the important quality parameters of soy sauce, including amino nitrogen content, ...     

Discrimination of herbal medicines by molecular spectroscopy and chemical pattern recognition

The molecular spectroscopy (including near infrared diffuse reflection spectroscopy, Raman spectroscopy and infrared spectroscopy) with OPUS/Ident software was applied to clustering ginsengs according to species and processing methods. The results demonstrate that molecular spectroscopic analysis could provide a rapid, nondestructive and reliable method for identification of Chinese traditional medicine. It's found that the result of Raman spectroscopic analysis was the best one among these three methods. Comparing with traditional methods, which are laborious and time consuming, the molecular spectroscopic analysis is more effective.     

现场制备的起爆炸药(EIS)的结构剖析

组成;现场制备的起爆炸药(EIS)的结构剖析     

Generalized two-dimensional correlation spectroscopy

Since the theory of generalized two-dimensional (2-D) correlation spectroscopy was proposed, it has been keenly concerned in scientific research and its analytical method has been widely applied in various analytical fields. The mathematical process to construct generalized 2-D correlation spectroscopy and the physical meaning of 2-D correlation spectral map are described, and three examples in the fields of chemical analysis and molecular biology are provided, such as the component analysis of organic solvent, the analysis of biological molecules in the solvent with different pH values and structural analysis of protein. The theory and analytical method of generalized 2-D correlation spectroscopy are also detailedly commented.     

Generalized two-dimensional correlation spectroscopy——Theory and applications in analytical field

After correlation analysis for general spectro- scopy, two-dimensional (2-D) correlation spectroscopy is obtained by extracting the information contained in the spectra in two dimensions, which is the function of two dependent spectral variables. 2-D correlation spectroscopy is initially regarded as an analytical data treatment method in the study of molecular interaction by using sinusoidal infrared sign[1]. In 1993, it was extended to generalized 2-D correlation spectroscopy, which used mo…     

Generalized two-dimensional correlation spectroscopy-- Theory and applications in analytical field

Since the theory of generalized two-dimensional (2-D) correlation spectroscopy was proposed, it has been keenly concerned in scientific research and its analytical method has been widely applied in various analytical fields. The mathematical process to construct generalized 2-D correlation spectroscopy and the physical meaning of 2-D correlation spectral map are described, and three examples in the fields of chemical analysis and molecular biology are provided, such as the component analysis of organic solvent, the analysis of biological molecules in the solvent with different pH values and structural analysis of protein. The theory and analytical method of generalized 2-D correlation spectroscopy are also detailedly commented.     

An antitumor agent of beta-cyclodextrin-modified titanocene complex: synthesis and characterization

The complex of a derivative of beta-cyclodextrin, that is mono[6-deoxy-6-(2-butenedinitrile-2,3-dimercapto sodium salt)]-beta-cyclodextrin (6-mnt-beta-CD), with titanocene (titanocene di[mono[6-deoxy-6-(2-butenedinitrile-2,3-dimercapto)]-beta-cyclodextrin], Cp2Ti[6-mnt-beta-CD]2) has been synthesized and characterized by IR spectroscopy, UV spectroscopy, elemental analysis, thermogravimetry, 1H- and 13C-NMR spectroscopy. The stoichiometry of the target molecule was determined by 1H-NMR spectroscopy and elemental analysis.     

藏药诃子质量标志物诃子酸的分离分析及标准化研究

依据GB/T 15000—2008《标准样品工作导则》的要求,研制诃子酸国家标准样品.以诃子的干燥成熟果实为原料,采用大孔吸附树脂、制备型高效液相色谱技术对标准样品进行制备,经过纯度分析、结构鉴定、均匀性检验、稳定性检验,最后进行联合定值.基于高效液相色谱(HPLC)技术,采用不同检测波长进行纯度测试,样品纯度均大于98%.基于液相-质谱(LC-MS)进行纯度分析,未发现明显杂质峰.通过紫外光谱(UV)、红外光谱(IR)、质谱(MS)、核磁共振(NMR)等技术确定其结构为诃子酸.样品均匀性良好,4℃条件下24个月内稳定性良好.定值结果确定诃子酸纯度为98.08%,在95%置信区间范围内的相对扩展不确定度为0.50%.研制出的诃子酸(GSB 11-3725-2020)国家标准样品可用于含量测定、检测方法评定、相关产品的检测与质量控制.     

Solid-phase glycosylation of peptide templates and on-bead MAS-NMR analysis: perspectives for glycopeptide libraries

The efficient solid-phase glycosylation of amino acid side chains (serine (Ser), threonine (Thr), and tyrosine (Tyr)) in peptides was demonstrated with a variety of glycosyl trichloroacetimidate donors in high yields and purities. A novel photolabile linker, with no chiral centre, was introduced to facilitate analysis by both matrix-assisted laser desorption ionisation time of flight (MALDI-TOF) mass spectrometry and nanoprobe magic angle spinning (MAS) NMR spectroscopy. Product analysis by nanoprobe MAS NMR spectroscopy, LC-MS and MALDI-TOF mass spectrometry of the glycosylation reactions indicated that the reactivity order of the hydroxy side-chain functions of amino acids in peptides on the solid-phase was Tyr>Ser>Thr. The nearly quantitative glycosylation yields and the efficient on-bead product analysis by nanoprobe MAS NMR spectroscopy have made a truly solid-phase approach for the synthesis and analysis of glycopeptide libraries possible.     

Raman spectroscopic study of the uranyl sulphate mineral zippeite: low wavenumber and U–O stretching regions

The uranyl sulphate mineral zippeite was studied by Raman spectroscopy. The phase purity of the sample was initially checked by X-ray powder diffraction and its chemical composition was defined by electron microprobe (wavelength dispersive spectroscopy, WDS) analysis. The Raman spectroscopy research focused on the low wavenumber and uranyl stretching vibration regions. Vibration bands down to 50 cm^–1 were tentatively assigned. The U–O bond lengths were calculated based on empirical relations. Inferred values are consistent with those obtained from the crystal structure analysis of synthetic zippeite. Number of bands was interpreted on the basis of factor group analysis.