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1.
高效液相色谱中的纤维素衍生物手性固定相   总被引:7,自引:0,他引:7  
李兵  施介华  杨根生 《化学通报》2003,66(3):169-173
评述了高效液相色谱中纤维素衍生物手性固定相直接拆分对映体的进展,介绍了纤维素衍生物的主要类型,纤维素衍生物作手性固定相三种不同方式的特点以及新的纤维素衍生物手性固定相应用,并结合色谱,NMR和分子模型设计和理论计算等方法讨论了纤维素衍生物手性固定的拆分机理。  相似文献   

2.
高效液相色谱中乙基纤维素手性固定相研究   总被引:1,自引:2,他引:1  
对映异构现象广泛存在于自然界中,由于对映异构体分子之间具有不同的光学性能和生物活性,因而外消旋体的拆分在药学和生物学等领域具有十分重要的意义.在手性拆分中,高效液相色谱是最普遍使用的方法之一,而其中又以手性固定相法最为常用[1].在众多手性固定相中,各种多糖及其衍生物,特别是纤维素和直链淀粉的衍生物因具有很好的手性识别能力而得到了广泛研究[2-3].但到目前为止,我们还未见乙基纤维素手性固定相的报道.本文制备了乙基纤维素手性固定相,并在正相、反相以及极性有机溶剂的流动相条件下,对15种手性化合物的拆分情况进行了探究,其中9种得到了不同程度的分离,研究结果表明该手性固定相具有较好的手性拆分能力.  相似文献   

3.
高效液相色谱蛋白质手性固定相   总被引:4,自引:0,他引:4  
本文综述了近年文献中已报道的各种高效液相色谱蛋白质(酶)手性固定相及其在手性拆分中的应用,并阐述了蛋白质作为手性选择剂拆分机理的研究进展。  相似文献   

4.
高效液相色谱手性聚合物固定相的研究与进展   总被引:2,自引:0,他引:2  
对近年来高效液相色谱手性固定相的研究进行了综述。重点介绍了手性聚合物固定相的分类和应用的新进展。讨论了各类手性固定相优缺点,提出了目前存在的问题和今后研究的方向和重点。  相似文献   

5.
张欣  高连勋 《分析化学》2001,29(5):526-529
合成了3种纤维素衍生物并分别填充分析型色谱柱,研究了不同的涂敷条件对柱效的影响以及色谱柱的稳定性,对外消旋化合物进行了手性拆分。实现了高效液相色谱-旋光仪的联用,获得了在线旋光曲线。  相似文献   

6.
纤维素衍生物手性固定相研究进展   总被引:1,自引:0,他引:1  
何永祝  庞浩  廖兵 《化学进展》2006,18(7):957-965
本文从用作手性固定相的纤维素衍生物种类、纤维素衍生物手性固定相制备方法及其在高效液相色谱中的应用三个方面介绍了国内外近年来的研究进展,并展望了该领域今后的研究方向。  相似文献   

7.
纤维素衍生物手性固定相研究进展   总被引:1,自引:0,他引:1  
本文从用作手性固定相的纤维素衍生物种类、纤维素衍生物手性固定相制备方法及其在高效液相色谱中的应用三个方面介绍了国内外近年来的研究进展, 并展望了该领域今后的研究方向.  相似文献   

8.
本文从用作手性固定相的纤维素衍生物种类、纤维素衍生物手性固定相制备方法及其在高效液相色谱中的应用三个方面介绍了国内外近年来的研究进展,并展望了该领域今后的研究方向。  相似文献   

9.
合成了纤维素-三(苯甲酯)(CTB)和纤维素-三(氨基苯甲酸酯)(CTPC)衍生物,并涂敷于自制的球形硅胶上(5μm,13nm),制备了用于高效液相色谱手性拆分的固定相.考察了涂敷量、流动相等因素对手性拆分的影响,测定了一个不对称氢化酯化反应的对映体过剩值(e.e.值).  相似文献   

10.
合成了一种经环十二烷修饰的纤维素酯,将其涂敷于小粒径的氨丙基化硅胶(APS)上,制备出高效液相色谱手性固定相,以正己烷、异丙醇为流动相拆分了2-对氯苯基丙腈、1-对氟苯基乙醇、1-对叔丁基苯氧基-2-丙醇、2-对氯苯基辛腈及三唑醇等5种外消旋对映体,并考察了流动相中异丙醇含量对分离效果的影响。  相似文献   

11.
Twenty different tris(phenylcarbamate)s of cellulose were synthesized and evaluated as chiral stationary phases for HPLC. Optical resolving power of the tris(phenylcarbamate)s depends on the substituents introduced on the phenyl groups. Optical resolving abilities of amylose tris(phenylcarbamate)s were also evaluated. In most cases, either cellulose tris(3,5-dimethylphenylcarbamate) or amylose tris(3,5-dimethylphenylcarbamate) exhibited the highest optical resolving ability. Aralkylcarba-mates such as benzyl- and 1-phenylethylcarbamates of cellulose and amylose were also tested as chiral stationary phases. (S)-1-Phenylethylcarbamate of amylose showed a high optical resolving power.  相似文献   

12.
Summary The reversed phase chromatographic properties of the [G1]-L-glutamic and ethyl ester-AC-silica (1), [G2]-L-glutamic acid ethyl ester-AC-silica (2) and the [G1]-L-glutamic acidt-butyl ester-AC-silica (3) dendrimer stationary phases were evaluated. Initial studies involved the comparison between these phases with a classic reversed phase (i.e. ODS1) by the separation of a standard reversed phase test mixture composed of dimethylphthalate, nitrobenzene, anisole, diphenylamine and fluorene. Separations were achieved with comparable performance to those obtained with the conventional reversed phase (ODS1). However, it was apparent that the chromatographic selectivity exhibited by the dendrimer stationary phases was different from that of the ODS1 phase. On a per mole basis, the dendrimers exhibited similar (and sometimes greater) affinity for these analytes compared with the ODS1 ligand. Subsequent chromatographic experiments were conducted upon the dendrimer chiral stationary phases using chiral analytes under reversed phase and normal phase conditions. Chiral resolution was not observed.  相似文献   

13.
Synthetic, optically active polymers used as CSP are reviewed. The polymers are classified into three major categories, namely, addition polymers, condensation polymers, and cross-linked gels. The emphasis lies on polymethacrylates having helical conformation belonging to the first category. Helical polymethacrylates are synthesized using asymmetric anionic or radical polymerization techniques and show resolving ability towards a wide range of racemate.  相似文献   

14.
环糊精类高效液相色谱固定相的研究进展   总被引:12,自引:0,他引:12  
陈慧  王琴孙 《色谱》1999,17(6):533-538
对高效液相色谱中的β-环糊精及其衍生物手性固定相的发展过程进行了综述,53篇。  相似文献   

15.
The interconverting stereoisomers of tri-o-thymotide have been separated by HPLC on chiral stationary phases and the temperature dependence of the dynamic chromatographic patterns has been interpreted in terms of exchange between enantiomeric propeller and helical conformations. Computed low energy structures and CD spectra were used in absolute configuration assignment.  相似文献   

16.
17.
Two hybrid polyacrylamide chiral stationary phases (CSPs) for HPLC have been synthesized by a new surface-initiated photo-induced radical polymerization approach of enantiopure N,N'-diacryloyl derivatives of (1R,2R)-diaminocyclohexane (CSP1) and (1R,2R)-diphenylethylenediamine (CSP2). This system is based on the activation of mesoporous silica microparticles by chemically bonded trichloroacetyl groups and dimanganese decacarbonyl as catalyst. UV irradiation was performed using a lab-made quartz photochemical reactor, ad hoc designed for the photo-induced polymerization process on the surface of microparticles. The two phases were evaluated and compared as chromatographic supports for the enantioselective HPLC of model chiral compounds. Their physico-chemical properties and chromatographic performances were also evaluated in comparison with those exhibited by the homologue CSPs obtained by the grafting-from thermal-induced process (CSP3 and CSP4). The new photopolymerization approach yielded higher grafting density than the thermal-induced one, especially in the case of the less reactive monomer (the diacryloyl derivative of (1R,2R)-diphenylethylenediamine), good chromatographic efficiency and a broad application field under normal phase and polar organic mode conditions.  相似文献   

18.
Cyclofructans (CF) are cyclic oligosaccharides consisting of a crown ether core with pendent fructofuranose units. These unique macrocycles were reported recently to be powerful chiral selectors. Derivatized and bonded to silica, CFs make excellent chiral selectors for HPLC. In this study, several new derivatives of cyclofructan 6 (CF6) were prepared by introducing aromatic moieties with electron-withdrawing chloro and nitro groups and an electron-donating methyl group. Their enantioselectivities were evaluated in the normal phase mode in comparison to the commercially available cyclofructan columns (LARIHC CF6-P, LARIHC CF6-RN, and LARIHC CF7-DMP). In several cases, the columns prepared in this work showed improved enantioselectivity over the existing commercially available stationary phases. Furthermore, an evaluation of the number and position of chloro and methyl groups on the phenyl substituents of CF6 is discussed in terms of their ability to alter enantioselectivity.  相似文献   

19.
Chiral stationary phases were synthesized and their ability to separate racemic precursors from which they were derived was assessed. Taken in conjunction with homochiral recognition previously observed in the solid state, the results of this study reveal that a geometrically controlling π-π interaction has a profound influence on molecular recognition.  相似文献   

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