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1.
刘振坤  杨波  廖霞俐  张淼  杨霞 《光谱实验室》2012,29(5):2630-2633
环糊精键接物具有直盲肠靶点释放性.通过使用羰基二咪唑(CDI)方法高产率的将丁酸键接到环糊精上,制备丁酸-a,β,γ-环糊精酯.对化合物进行了结构鉴定,并与合成该化合物的另一方法进行了对比.  相似文献   

2.
应用光谱分析技术研究碘与β-环糊精结合物的结构特征   总被引:3,自引:0,他引:3  
本文应用傅里叶变换拉曼光谱、傅里叶变换红外光谱、紫外光谱等分析方法,对采用不同工艺制备的碘与β-环糊精结合物进行了定性、定量分析。研究发现,碘与β-环糊精结合中碘的存在形式为游离碘、包结碘和胶束络合碘。水法工艺制备的样品,含碘量高但稳定性差。醇法工艺制备的样品,含碘量低而稳定性好。本实验建立的检测碘与β-环糊精结合物的分析方法简便易行,实验取得了满意的效果,本方法可用于制备碘与β-环糊精结合物原料药的质量控制。  相似文献   

3.
用顺丁烯二酸酐(MAH)对β-环糊精(β-CD)进行化学改性,合成出了顺丁烯二酸酐-β-环糊精衍生物(MAH-β-CD)。针对影响衍生物制备的因素,采用正交实验法,以产物产率为评价指标,优选顺丁烯二酸酐-β-环糊精衍生物制备的最佳工艺条件为:投料比1∶10,反应温度80℃,反应时间9h。  相似文献   

4.
采用旋转甩涂法在钾离子(K+)交换玻璃光波导表面制备了聚乙烯吡咯烷酮(PVP)-环糊精复合薄膜,研制了PVP-环糊精薄膜/K+交换玻璃光波导传感元件,并对挥发性有机气体进行了检测。该气敏元件对苯乙烯和二甲苯具有较好的响应,并能够检测到体积比为1×10-6的苯乙烯和1×10-5的二甲苯。还具有响应及恢复速度快、容易制备等特点。  相似文献   

5.
通过FT-IR(傅里叶变换红外光谱)和Raman(共焦激光拉曼光谱)分析黄芩苷包合物,对拉曼光谱法作为一种新的验证包合物形成方法的可行性进行验证.采用饱和水溶液法制备黄芩苷包合物,共焦拉曼光谱仪和傅里叶转换红外光谱仪分别测定并获得p-环糊精、黄芩苷、黄芩苷与β-环糊精物理混合物及黄芩苷包合物四种固体粉末的拉曼图谱和红外...  相似文献   

6.
制备了以β-环糊精为主体,荧光黄为客体的晶体包合物,用红外光谱、DSC曲线、荧光光谱、共振瑞利散射光谱等方法确定了包合物的形成,对包合物的形成进行了初步讨论,并用Hildebrand-Benesi双倒数法测定了包合物的包合常数.实验结果表明:β-环糊精与荧光黄分子形成包合比为1:1的包合物.  相似文献   

7.
连翘酯苷/β-环糊精包合物稳定性研究   总被引:1,自引:0,他引:1  
马运萍  李鹏鸽 《光谱实验室》2009,26(5):1219-1222
用饱和溶液法制备了β-环糊精与连翘酯苷的包合物,荧光光谱法对包合物进行了表征。测定了包合物的形成常数及其在293-328K范围内的热力学参数△G、△H、△S。实验表明:包合过程是一个放热过程。连翘酯苷经β-环糊精包合后提高了稳定性,具有一定程度的抗氧化、抗光解性。  相似文献   

8.
β-环糊精与佐匹克隆包合作用的研究   总被引:2,自引:1,他引:1  
采用相溶解度法研究了佐匹克隆在不同pH和不同摩尔浓度的β-争环糊精水溶液中的溶解度及二者的表观稳定常数,随着β-环糊精浓度的增加和pH的提高,佐匹克隆的溶解度增加,表观稳定常数升高;采用热力学方法研究了温度对包合反应的影响,计算了包合过程的熵变AS、焓变△H及自由能变化△G均为负值,说明包合反应是放热反应且能自发进行,焓变是形成超分子复合体的主要驱动力;用研磨法制备了佐匹克隆-环糊精包合物,并用红外光谱和差示扫描量热分析对固体包合物进行了表征.结果表明,佐匹克隆与β-环糊精可形成1:1包合物,β-环糊精对于难溶性药物佐匹克隆是较理想的增溶剂.  相似文献   

9.
制备了一种羧基-β-环糊精衍生物,并将它包络二茂铁,制得了二茂铁-羧基-β-环糊精包络物,用红外光谱、紫外可见光谱、1HNMR、13CNMR等方法表征了羧基-β-环糊精及二茂铁包络物。由于羧基-β-环糊精衍生物破坏了β-环糊精的分子内氢键,并修饰了羧基,使得其水溶性得到明显的提高。研究了包络物的电化学性质,发现其具有良好的氧化还原可逆性和水溶性,可用作电子传递媒介体,循环伏安法测定表明,其检出限为10-7mol/L,表明这类氧化还原具有很高的灵敏度,可以用作性能优异的电化学探针和电流型生物传感器的电子媒介体。  相似文献   

10.
阿维菌素包合物的红外光谱研究   总被引:1,自引:0,他引:1  
依据β-环糊精的分子空腔容纳性质,利用饱和水溶液法制备出阿维菌素-β-环糊精包合物,利用高效液相色谱法测定其包封率。结合红外光谱谱图说明了阿维菌素-β-环糊精包合物的形成;分析了阿维菌素光解所产生的化学结构变化;研究了所形成的包合物增强阿维菌素化学结构光稳定性的效应。结果表明:阿维菌素-β-环糊精包合物的包封率为40.5%;从红外光谱谱图分析,说明阿维菌素-β-环糊精包合物形成了分子间氢键,组合效应与其物理混合物有区别。阿维菌素B1a分子大环内酯结构可以被光分解破坏,分解后大环内酯结构中的C—O—C结构红外伸缩振动峰消失,内酯键发生明显断裂。形成阿维菌素-β-环糊精包合物后,β-环糊精起包合作用的分子位点覆盖了阿维菌素B1a分子大环内酯结构,为阿维菌素B1a分子大环内酯结构中的C—O—C结构提供良好的避光保护作用,提高了阿维菌素B1a分子的光稳定性。本实验的创新之处在于对所制备的阿维菌素-β-环糊精包合物的结构和特性从红外光谱角度进行了分析,此类包合物可望作为理想的阿维菌素保护型控释制剂中间体。  相似文献   

11.
环糊精包合作用及其分子识别功能的研究进展   总被引:4,自引:0,他引:4  
本文介绍了环糊精超分子化学领域的研究概况,从环糊精的包合作用及其分子识别功能两个方面进行了简要概述。  相似文献   

12.
Summary Polyamines and polyamine conjugates display a diverse range of important biological functions, ranging from antibiotics to immunosuppressants and glutamate receptor antagonists. For these reasons, polyamines provide an excellent template/scaffold for combinatorial chemistry. In this paper we present methods for the solid-phase immobilisation of polyamines for use in synthetic and combinatorial chemistry and describe how they have been employed in the preparation of a number of important polyamine conjugates and polyamine libraries. Thus, we have designed, synthesised and utilised a number of polyamine linkers for both solution and resin screening combinatorial application.  相似文献   

13.
In the work the focus is on the preparation of self-assembled monolayer-like films consisting of thiolated cyclodextrin on gold substrate and a characterization by using secondary ion mass spectrometry. The short (1 min) and long (1 h) time preparations of self-assembled monolayer-like films, resulting in submonolayer and monolayer regimes, are investigated, respectively. The observed species of thiolated cyclodextrin (M as molecular ion) self-assembled monolayer-like films are assigned to three groups: AuxHySz clusters, fragments with origin in cyclodextrin molecule associated with Au, and molecular ions. The group of AuxHySz (x = 2-17, y = 0-2, z = 1-5) clusters have higher intensities than other species in the positive and even more in negative mass spectra. Interestingly, the dependence between the number of Au and S atoms shows that with the increasing size of AuxHySz clusters up to 11 Au atoms, the number of associated S atoms is also increasing and then decreasing. Molecular species as (M−S+H)Na+, (M+H)Na+, AuMNa+, (M2−S)Na+, and M2Na+ are determined, and also in cationized forms with K+. The intensities of thiolated cyclodextrin fragments at the long time preparation are approximately 10 times higher than the intensities of the same fragments observed at the short time. The largest observed ions in thiolated cyclodextrin self-assembled monolayer-like films are AuM2 and Au2M. The thiolated cyclodextrin molecular ions are compared with hexadecanethiol molecular ions in the form of AuxMw where the values of x and w are smaller for thiolated cyclodextrin than for hexadecanethiol. This result is supported with larger, more compact, and more stabile thiolated cyclodextrin molecule.  相似文献   

14.
Summary A combinatorial library containing mixtures of amides and esters was prepared through solid-phase chemistry. The advantages of using solid-phase chemistry over solution-phase chemistry to prepare this library are discussed. The library was screened through a high-throughput whole organism herbicidal assay upon which a mixture containing amides was found to have herbicidal activity. Deconvolution of the mixture providedN-(3-benzoylphenyl)-3-(1,1-dimethylethyl)-1-methyl)-1H-pyrazole-5-carboxamide as a herbicidal lead with broadleaf and narrowleaf pre-emergence herbicidal activity as low as 100 g/ha on some weed species. This study represents the first report of an agrochemical discovered using a combinatorial approach. Supplementary Material, comprising experimental procedures for the preparation of resin II and the reaction of II with nucleophiles, GC/MS and LC/MS data for the reaction ofII with morpholine, and a detailed experimental for the preparation of 2 with characterization data, is available upon request.  相似文献   

15.
The preparation of solid supported glycine phosphonate and its utilization for the total synthesis of two natural products is presented. The proposed protocol combines diversity with accessibility and speed, which makes this scaffold suitable for automated parallel synthesis and combinatorial chemistry. The preparation of a small library of dehydro-2,5-diketopiperazines, combining several natural amino acids with diverse heterocycles (including thiazoles, pyridines, indoles and imidazoles), is also demonstrated.  相似文献   

16.
The use of solution phase techniques has been explored as an alternative to solid-phase chemistry approaches for the preparation of arrays of compounds in the drug discovery process. Solution-phase work is free from some of the constraints of solid-phase approaches but has disadvantages with respect to purification. This article will also illustrate some of the advances made in recent years in solution phase array chemistry including using supported reagents and simple extractive protocols for the effective preparation of high quality samples.  相似文献   

17.
表面增强拉曼光谱(SERS)作为一种快速、灵敏的分析技术,被广泛应用于分析化学、环境检测及食品安全等领域。在实际生活中的样品大多为混合物,直接使用SERS技术无法对复杂样品中的分析物进行准确测定。薄层色谱(TLC)分离技术具有操作简便,成本低廉及分离速度快等特点,TLC作为一种高通量的分离技术在合成化学、分析化学、药物化学及食品科学等研究领域得到了广泛的应用。TLC对待测物体系进行分离后,通过碘显色或荧光对分离的斑点进行可视化处理,再结合质谱,红外光谱、荧光光谱及SERS光谱等分析技术可以对分离物质进行定性及定量分析。TLC与SERS联用技术的出现,使得SERS光谱可以应用于混合物中分析物的有效测定。TLC-SERS技术同时具备良好的分离作用和灵敏的光谱检测性能,适用于对复杂样品进行分离检测。在TLC-SERS检测过程中,样品用量少且无需使用复杂的实验设备即可实现对混合物现场快速检测。介绍了SERS的增强机理以及活性基底的制备,对TLC-SERS技术在环境污染物检测、食品安全、中草药鉴定及生物医学等方面的应用做了概括性综述。给出了TLC-SERS技术在有害物快检领域的应用实例,为TLC-SERS技术未来用于食品安全、法医鉴定及环境治理中快速检测方法建立及仪器设备研发提供参考。  相似文献   

18.
Solutions of alpha, beta, and gamma cyclodextrin have been shown to enhance the chemiluminescence of the reaction between hydrogen peroxide and 10,10'-dimethyl-9,9'biacridinium nitrate. A 20-fold increase in chemiluminescence intensity is observed in 10-2 M beta cyclodextrin. The enhancement is attributed to an increase in the excitation efficiency and the rate of the reaction through the inclusion of a reaction intermediate in the cyclodextrin cavity.  相似文献   

19.
研究了在异丙醇-硝酸体系中单次分子镀流程制备Sm和Eu厚靶的实验条件。确定了在20 μm铍箔上进行Sm和Eu分子镀实验的最佳工艺条件为: 两极间距3 cm, 电流密度3.8mA/cm2, 分子镀过程持续1h。 用分光光度法测定了分子镀的沉积效率均高于95%, 所制备Sm和Eu靶膜的厚度分别在1.6和1.5 mg/cm2。  相似文献   

20.
Cyclodextrin-based aggregates and characterization by microscopy   总被引:2,自引:0,他引:2  
Cyclodextrin-based aggregates have been widely investigated with microscopies such as STM, AFM, SEM, TEM, and fluorescent microscopy to obtain the direct morphology and structure of samples. In the present review, we discuss various types of cyclodextrin aggregates, that is, native and modified cyclodextrins, inclusion complexes and their aggregates of cyclodextrins, cyclodextrin rotaxanes and polyrotaxanes, cyclodextrin nanotubes and their secondary assembly, and other high-order aggregates of cyclodextrins. Especially, we focus on the use of microscopy to characterize above aggregates. The application of modern microscopy tools promotes the investigation on cyclodextrins.  相似文献   

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