共查询到17条相似文献,搜索用时 140 毫秒
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高效液相色谱(HPLC)被广泛认为是分离制备光学纯单一对映体的最有效方法。在高效液相色谱手性拆分中,手性固定相(CSP)的性能直接影响到色谱柱的手性分离能力。在众多手性固定相中,键合型手性固定相具有溶剂耐受性好,分离模式灵活等优点,已经发展成为一类重要的手性固定相。本文通过两步化学反应合成了新型的光学活性丙烯酰胺衍生物--(S)-1-丙烯酰-2-(N-苯基甲酰胺基)吡咯烷((S)-APACP),采用核磁共振氢谱表征了(S)-APACP的化学结构;通过3步化学反应制备了键合型聚丙烯酰胺衍生物手性固定相,采用热重分析法表征了聚合物的键合量,采用HPLC评价了键合型手性固定相的识别能力,分析了影响其手性识别能力的因素。研究结果表明,APACP聚合物成功地键合到硅胶表面制备了具有良好溶剂耐受性的键合型手性固定相,其聚合物键合量为10.2%~11.8%,该键合型手性固定相对若干种对映体显示了较好的手性识别能力。 相似文献
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多糖衍生物类固定相在高效液相色谱手性分离中的应用进展 总被引:3,自引:0,他引:3
评述了多糖衍生物手性固定相在高效液相色谱手性分离中的应用进展,介绍了多糖衍生物手性固定相的主要类型,阐述了手性拆分机理和影响手性拆分的因素,引用文献66篇。 相似文献
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高效液相色谱蛋白质手性固定性 总被引:1,自引:0,他引:1
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
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键合偶联双奎宁手性固定相的制备和手性拆分性能;手性固定相;奎宁;高效液相色谱;拆分 相似文献
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Summary The chromatographic separation and resolution of the enantiomers of flurbiprofen and its two major metabolites, 4′-hydroxyflurbiprofen
and 3′-hydroxy-4′-methoxyflurbiprofen was investigated using four different approaches: reversed-phase HPLC after pre-column
derivatization with (R)-1-(naphthen-1-yl)ethylamine; reversed-phase HPLC using hydroxypropyl-β-cyclodextrin as a chiral mobile phase additive; chiral-phase
HPLC using either an α1-acid glycoprotein CSP (Chiral-AGP) or an amylose tris(3,5-dimethylphenylcarbamate) CSP (Chiralpak AD). Of all the approaches,
only the direct method using the Chiralpak AD CSP demonstrated separation and enantiomeric resolution of all three analytes
within an acceptable run time of 45 minutes. Enantiomeric resolution values of 1.67,3.67 and 3.44 were obtained for flurbiprofen,
4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen respectively. Semi-preparative isolation of the individual enantiomers
of both metabolites, followed by CD analysis, revealed that the elution order on the AD CSP wasR-beforeS-enantiomer for both metabolites and the same as that observed for flurbiprofen. The metabolite elution order was subsequently
confirmed on the analysis of urine samples obtained from a healthy volunteer following oral administration of the individual
drug enantiomers. 相似文献
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Amylose tris-(S)-1-phenylethylcarbamate chiral stationary phase (CSP) was prepared. The direct enantiomeric separation of chiral pesticides on this CSP had been studied by HPLC. The mobile phase was n-hexane-isopropanol at a flow rate of 1.0 mL/min. The effects of isopropanol content and column temperature on retention and enantioselectivity were investigated. Thirty-two samples were tested, of which ten interacted enantioselectively with the CSP. Five samples were completely resolved and another five underwent near-baseline or partial resolution. The enantiomers were identified by a circular dichroism detector. Linear van't Hoff plots were established and the thermodynamic parameters were thus calculated. 相似文献
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Helical polymers have attracted a great deal of attention and been extensively investigated due to their various applications.One of the most important applications of helical polymers is chiral recognition and resolution of enantiomers for the reason that a pair of enantiomers is commonly with different physiological and toxicological behaviors in biological systems.Helical polymers usually present unexpected high chiral recognition ability to a variety of racemic compounds.What's more,the chiral recognition and resolution abilities of the system are dependent on the highly ordered helical structures of the helical polymers.This mini review mainly focuses on the recent progress in chiral recognition and resolution based on helical polymers.The synthetic methodology for helical polymers is firstly discussed briefly.Then recent advances of chiral recognition and resolution systems based on helical polymers,especially polyacetylenes and polyisocyanides,are described.We hope this mini review will inspire more interest in developing helical polymers and encourage further advances in chiral-related disciplines. 相似文献
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Two chiral stationary phases (CSPs) based on optically active (3,3′-diphenyl-1,1′-binaphthyl)-20-crown-6 covalently bonded to silica gel were utilized for the first time for the resolution of racemic β-amino acids using high performance liquid chromatography. All of the 10 β-amino acids tested were resolved on the CSP containing residual silanol-protecting n-octyl groups, while only five β-amino acids were resolved on the CSP containing residual silanol groups. The superiority of the CSP containing residual silanol-protecting n-octyl groups and the characteristic retention behaviors of the two enantiomers on the CSP were rationalized to stem from the removal of the residual silanol groups, which can otherwise induce the non-enantioselective retention of the analytes, and the improved lipophilicity of the CSP. The elution orders of the two enantiomers of β-amino acids were identical on the two CSPs and, consequently, it was concluded that the two CSPs were concluded to utilize identical chiral recognition mechanisms. The different elution orders of the analytes were proposed to be attributed to the presence or absence of π-π interactions between the CSP and analytes. 相似文献
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Rifamycin-capped (3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles (RCD-HPS), a new type of substituted β-cyclodextrin-bonded chiral stationary phase (CSP) for high-performance liquid chromatography (HPLC), have been synthesized by the treatment of bromoacetate-substituted-(3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles (BACD-HPS) with rifamycin SV in anhydrous acetonitrile. The stationary phase is characterized by means of elemental analysis and Fourier-transform infrared spectroscopy. This new CSP has a chiral selector with two recognition sites: rifamycin and β-cyclodextrin (β-CD). The chromatographic behavior of RCD-HPS was studied with several disubstituted benzenes and some chiral drug compounds under reversed-phase HPLC mobile phase conditions. The results show that RCD-HPS has excellent selectivity for the separation of aromatic positional isomers and enantiomers of chiral compounds due to the cooperative functioning of rifamycin and β-CD. 相似文献