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基于高压制备液相的多维色谱技术在中药分离纯化中的应用 总被引:1,自引:0,他引:1
中药物质基础复杂,对其活性成分的分离一直是中药研究的难题.基于高压制备液相的多维色谱系统在高压制备液相色谱的基础上,结合了多种分离技术,极大地提高了色谱系统的分离性能和分离效率,更有利于对物质基础复杂的中药样品进行分离纯化.本文介绍了基于高压制备液相系统的多维色谱系统的基本原理、分离模式以及关键技术,并综述了其在中药分离纯化中的应用. 相似文献
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1 多维分离技术新进展
一维色谱是目前最常用的分离分析方法,然而对于复杂体系如蛋白质组,采用一维分离模式其分离度远远不能满足要求.Giddings理论告诉我们:对于分离机理相互正交的二维分离系统(如色谱),峰的容量应该为两个色谱柱峰容量的乘积.因此,多维分离系统是解决复杂分离体系的一个最佳选择.在多维色谱中二维气相色谱发展较快,目前全二维气相色谱仪业已商品化,其峰的容量达到104以上.而二维液相色谱,尤其是正相/反相二维液相色谱技术发展较为缓慢,其主要的技术瓶颈在于第一维色谱(正相)分离后的流动相严重干扰第二维色谱(反相)的分离. 相似文献
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金属-有机骨架材料(Metal-organic frameworks,MOFs),因其具有较好的热稳定性、化学稳定性、可设计性等特点,广泛应用于气体吸附、物质分离、提纯、催化等领域,同时也作为模板制备各种功能材料.MOFs作为色谱分离的材料已得到了较多的研究与应用.按照被分离物质的类别,综述和总结了不同MOFs材料作为色谱固定相的分离效果,重点介绍了MOFs材料的色谱分离机理.MOFs材料的孔径、功能基团和不饱和金属位点在分离中起到重要的作用,最后对MOFs在色谱分离应用中的问题和前景进行了分析和展望. 相似文献
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考察了烷基酚聚氧乙烯醚在反相色谱、正相键合色谱、硅胶吸附色谱、体积排阻色谱4种不同液相色谱分离模式中的分离效果,分别采用Kromasil C_(18)(250 mm× 4.6 mm,5 μm)、Agilent ZORBAX NH2(250 mm× 4.6 mm,5 μm)、Waters Spherisorb S3W(150 mm×2.0 mm,3 μm)和Shodex MSpak GF-310 2D(150 mm×2.0 mm,5 μm)色谱柱,以225 nm为紫外检测波长,对不同液相色谱分离模式的流动相组成、梯度洗脱条件、柱温、流速等进行了优化,并对烷基酚聚氧乙烯醚在不同液相色谱分离模式中的保留机理进行了初步探讨.结果表明,正相键合色谱实现了烷基酚聚氧乙烯醚的最佳分离;硅胶吸附色谱和体积排阻色谱的分离效果较正相键合色谱稍差. 相似文献
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Summary Poly(methyl-3-propylthiol)siloxane has been evaluated for use as stationary phase in open tubular columns for gas and supercritical fluid chromatography. Immobilization of the stationary phase was achieved by crosslinking with 2,4,6-trichloro-1,3,5-triazine. The poly(methyl-3-propylthiol)siloxane stationary phase film was in situ oxidized to the disulphide and sulphonic acid forms and both have been evaluated for use in supercritical fluid chromatography. Good selectivity towards polar polycyclic aromatic compounds has been shown. All the modified forms of the stationary phase were loaded with silver ions and were evaluated with regard to ligand exchange chromatography using supercritical fluid carbon dioxide as a mobile phase. The utility of the stationary phase, having sulphonic acid groups loaded with silver ions, has been demonstrated by separation of fatty acid methyl esters according to their unsaturation.Dedicated to Professor Leslie S. Ettre on the occasion of his 70th birthday. 相似文献
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Summary The chromatographic properties of an alkylphosphonate-modified magnesia-zirconia composite stationary phase have been investigated
by reversed-phase high-performance liquid chromatography with basic compounds as probes. The influence of organic modifier
composition and mobile phase pH was studied. The new stationary phase, similar to a silica-based reversed-phase stationary
phase, has hydrophobic properties, but greater pH stability. Use of the phase results in more symmetric peaks for basic compounds.
A possible mechanism of retention of basic solutes on the new stationary phase is discussed. The chromatographic behavior
of the basic solutes depends mainly on hydrophobic interactions between the solutes and the hydrophobic moiety of the stationary
phase. Br?nsted acidic and basic sites on the surface of the new stationary phase play an important role in the retention
of ionized solutes by ion-exchange interaction. Promising separations of some basic compounds have been achieved by use of
methanolic TRIS buffer, pH 10.0, as the mobile phase. 相似文献
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Roya Mohammadzadeh Kakhki 《Journal of inclusion phenomena and macrocyclic chemistry》2013,75(1-2):11-22
Recently, much attention has been paid to chromatographic characteristics and applications of crown ethers. These compounds were employed as chiral stationary phase for resolution of various racemic compounds in high performance chromatography and capillary electrochromatography techniques. Crown ethers also used in gas chromatography as the stationary phase. Recently, it has been found that, crown ethers also may be useful in cation chromatographic separation in ion chromatography for the determination of alkali and alkaline-earth cations, ammonium, and amines. In this paper we have an overview on these applications of crown ethers. 相似文献
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Summary The equation for the potential energy of interactions established for gas-liquid chromatography has been confirmed in reversed phase liquid chromatography. Equations derived for molecular polarizabilities of PAHs and their retention data have very high correlation coefficients. The results indicate that the inductive effect between solute and stationary phase is the main one and the dispersive effect is very small compared with the inductive effect but its contribution increases with the carbon chain length of the stationary phase. 相似文献
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The retention characteristics of alkylbenzenes and polycyclic aromatic hydrocarbons (PAHs) have been examined in liquid chromatography on a microcapillary column packed with cellulose acetate. Particulate and fibrous cellulose acetate were used as the stationary phase. Fibrous cellulose diacetate was found to be of use as an alternative stationary phase for liquid chromatography, although the separation efficiency was low. The retention characteristics for planar PAHs were linearly correlated with the size of the molecules, but the retention behavior for alkylbenzenes and nonplanar PAHs was affected by exclusion. The retention order was strongly influenced by the addition of dimethylformamide or water to methanol in the mobile phase. The results suggested that the retention behavior is influenced by a slight change in the polymer matrix of cellulose acetate. 相似文献
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A. N. Korol 《Theoretical and Experimental Chemistry》1967,1(6):516-520
The reaction of some simple molecules with polar and nonpolar stationary phases in gas-liquid chromatography has been examined. The important part played by the structure of the stationary phase in determining the form of the thermodynamic functions has been demonstrated. The individual elementary characteristics of the thermodynamic functions for dissolution in gas-liquid chromatography have been determined. 相似文献
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硅胶基质高效液相色谱填料研究进展 总被引:2,自引:0,他引:2
高效液相色谱(HPLC)不仅是一种有效的分析分离手段,也是一种重要的高效制备分离技术。色谱柱是HPLC系统的核心,不同性能的填料是HPLC广泛应用的基础。硅胶是开发最早、研究最为深入、应用最为广泛的HPLC固定相基质,其制备方法主要有喷雾干燥法、溶胶-凝胶法、聚合诱导胶体凝聚法及模板法等。近年来,亚2μm小粒径硅胶、核-壳型硅胶、双孔径硅胶、介孔性硅胶、有机杂化硅胶等新型硅胶应用于HPLC并取得了色谱分离技术的飞速发展,例如基于亚2μm填料的超高压液相色谱技术、基于核-壳型填料的快速分离技术、基于杂化硅胶填料的高温液相色谱技术等。硅胶经表面化学键合、聚合物包覆等有机改性可制得先进的大分子限进填料、温敏性填料、手性填料等,大大扩展了HPLC的应用范围。本文对液相色谱用硅胶的制备方法、改性与修饰方法以及硅胶基质固定相的评价方法加以系统综述,概述了新型硅胶在HPLC中的应用进展,并对硅胶基质填料的发展方向与应用前景进行了展望。 相似文献
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Ionic liquids (ILs) immobilized on silica as novel high performance liquid chromatography (HPLC) stationary phases have attracted considerable attention. However, it has not been applied to protein separation. In this paper, N-methylimidazolium IL-modified silica-based stationary phase (SilprMim) was prepared and investigated as a novel multi-interaction stationary phase charged positively for protein separation. The results indicate that all of the basic proteins tested cannot be absorbed on this novel stationary phase, whereas all of the acidic proteins tested can be retained, and the baseline separation of eight kinds of acidic protein standards can be achieved when performed in reversed phase/ ion-exchange chromatography (RPLC/IEC) mode. Compared with commonly used commercial octadecylated silica (ODS) column, the novel stationary phase can show selectivity and good resolution to acidic proteins, which has a promising application in the separation and analyses of acidic proteins from the complex samples in proteomics. In addition, the chromatographic behavior of proteins, the effect of the ligand structure and the retention mechanism on this stationary phase were also investigated. 相似文献