高效液相色谱烷基硅胶键合固定相

综述了高效液相色谱烷基硅胶键合固定相研究的最新进展,参考文献４０篇。     

苯胺甲基键合固定相的合成和色谱性能

多环芳烃;色谱法;苯胺甲基键合固定相的合成和色谱性能     

高效液相苯胺甲基键合硅胶固定相的保留机理研究

 制备了 3种不同键合量的苯胺甲基键合硅胶固定相 ,分别在正、反相条件下研究了它们对芳烃及其极性、酸性、碱性取代衍生物的保留和分离选择性 ,探讨了该固定相的保留机理 ,并考察温度对溶质在具有不同键合量的固定相上保留的影响。结果表明 :苯胺甲基键合硅胶固定相对溶质的保留是疏水、π π、偶极 偶极和电荷转移等多种作用的结果 ,在反相模式中 ,疏水作用对溶质的保留起主要作用。     

Separations in Thin Layer and High Performance Liquid Chromatography Using Alkyl Silica Gel Bonded Phases

Abstract

Separations in thin layer (TLC) and high performance liquid chromatography (HPLC) using alkyl bonded phases were carried out under optimum solvent conditions for each of three phases, RP-2, RP-8 and RP-18. The phases were tested for their efficiency and resolving power using three groups of compounds in three binary organic-water mobile phases. The organic solvents were acetonitrile, methanol and tetrahydrofuran, which are widely used as solvent modifiers in reversed phase liquid chromatography.

The results showed that, unlike HPLC, TLC using RP-18 plates was the most, and RP-2 plates the least, efficient. A naphthalene and biphenyl mixture which was resolved by HPLC using any of the three solvents and columns was not resolved by TLC using any plate or solvent combination, unless the plate was prewashed with an organic modifier. The addition of NaCl (1–2% wt/vol) to the solvent for TLC speeded development unless an alcohol was used, but did not greatly affect the separation.     

Non-Porous Silica Supports for High Performance Liquid Chromatography

Abstract

The physical and chromatographic properties of two types of non-porous HPLC support materials were examined. Loading capacities of non-porous supports were about 10 fold less than of wide-pore gels, while their physical strength was much greater, suggesting that non-porous supports could be useful for polymer separations. Such materials appeared to be less suitable for low-molecular-weight solutes, except for fundamental retention studies, where the absence of pore structure offers a less ambiguous support matrix.     

高效液相色谱环糊精键合固定相

环糊精是由Ｄ（＋）－葡萄糖单元通过α－１，４糖苷键连接的环状齐聚糖，其最典型的性质是能与许多客体分子形成包容配合物。高效液相色谱环糊精键合固定相广泛用于对映异构体，非对映异构体，结构异构体和常规化合物的分离。     

聚苯乙烯包夹硅基高效液相色谱固定相的研究

用包夹聚合法制备出一种新型的聚苯乙烯包夹硅基高效液相色谱固定相并进行了固定相的表征。对色谱行为的研究表明此固定相在分离碱性、强极性溶质时有良好的分离性能,固定相在较高ｐＨ的洗脱液中有较好的稳定性。     

硅胶基质高效液相色谱填料研究进展

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。     

高效液相色谱用硅质填料的进展

 对高效液相色谱用硅质填料的进展情况做了全面的评述。介绍了硅质填料的制备及化学修饰 ,评价了硅胶表面的物理表征 ,概括了硅质填料在高效液相色谱中的应用 ,并对我国的硅质填料前景进行了展望。     

Preparation and Evaluation of Calix[8]arene Bonded Silica Stationary Phase for High Performance Liquid Chromatography

In recent years, calix[n]arenes (n=4,5,6,7,8) as stationary phase have been introduced into the field of chromatography. In our previous works, we have synthesized, characterized and evaluated two different silica-bonded calix[n]arenes (n=4,6) stationary phase, on which the chromatographic behavior of PAHs, positional isomers,nucleosides and bases was investigated. In this paper we report the preparation of calix[8]arene bonded silica stationary phase, and characterization of its structure and chromatographic behavior.     

Application of Native and Hydroxypropyl-Substituted β-Cyclodextrin Bonded Silica Gel as Stationary Phases for High Performance Liquid Chromatography

Two chiral stationary phases for high-performance liquid chromatography (HPLC) have been synthesized by grafting native and 2-hydroxypropyl-β-cyclodextrin onto silica gel by a previously described method. They were tested under reversed-phase conditions. These two materials enable separation of the enantiomers of a variety of drugs (benzodiazepine anxiolytics, arylpropionic acids, anti-inflammatory and anticoagulant agents) and herbicides (aryloxyphenoxypropionic esters). Both chiral stationary phases enabled good chiral recognition in reversed-phase mode. The effects of the nature and composition of the mobile phase, of compound structure (mechanisms of chiral discrimination), and of flow-rate were studied.     

Preparation of Cibacron Blue F3GA Bonded Poly (styrenedivinylbenzene) (PSDVB) Microbeads Used for High Performance Affinity Chromatography

Recentlyhighperformanceliquidaffinitychr0mat0graphy(HPLAC)hasdevel0pedveryquickly.HPLACcombinesthespeedandres0lvingp0werofHPLCwithbiol0gicalspecificityofaffinitychromatographyandhasbeenwidelyusedasananalyticalt00linbiochemicalresearch.CibacronBIueF3GAisthem0stwideIyusedreactivetriazine-baseddyewhichhasspecificinteracti0nwithpyridinenucleotide-dependentdehydr0genase,kinase,blo0dproteinsandotherpr0teinsandenzymes'.ltisasuitabIeHPLACligandbecauseofitsreactivityandchemicaIstability.Inthi…     

高效液相色谱快速分离生物大分子的大孔硅质固定相的研制及应用

介绍了不同孔径的大孔硅胶基质的制备、二醇固定相的合成及其对蛋白质的色谱分离；考察了焙烧温度对硅胶孔隙度的影响；探讨了流动相中盐浓度和ｐＨ对蛋白质保留时间、柱效、分离度的影响以及硅胶孔径对键合密度和分离性能的影响。该种大孔固定相相对于常规多孔固定相具有小的比表面积、柱容量低、从而有利于生物大分子的微量分离分析。     

Effect of Alkyl Chain Length of Bonded Silica Phases on Separation,Resolution and Efficiency in High Performance Liquid Chromatography

Abstract

A comparative study of alkyl bonded phases was carried out under optimum solvent conditions for each phase. Three columns, RP-2, RP-8 and RP-18, were tested for their efficiency and resolving power using three groups of compounds in three binary organic-water mobile phases. The organic solvents were acetonitrile, methanol and tetrahydrofuran which are widely used as solvent modifiers.

The results indicate that each of the three factors, i.e. solvent, solute and bonded alkyl chain length, play an important role, with the solvent being the most significant. When tetrahydrofuran-water was used as the mobile phase, the ratio of THF/H₂O did not vary by much when an RP-2, RP-8 or RP-18 column was used to separate naphthalene from biphenyl, dimethylphthalate from diethylphthalate or anthraquinone from methyl, anthraquinone and ethyl anthraquinone. When acetonitrile-water and methanol-water were used the ratio of organic modefier to water changed so as to accomodate the hydrophobic properties of the columns. The efficiency of the columns, expressed as theoretical plates per meter (TPM) was highest when acetonitrile-water was used as the mobile phase. Although there were variations in TPM and resolution from column to column, the three columns gave good separation of the components of the three groups of compounds.     

高效亲和液相色谱法纯化基因重组人白细胞介素-2

1 引言高效亲和液相色谱(HPAC)是将经典亲和色谱的高特异性同高效液相色谱的快速、高效相结合产生的一种蛋白质的分离技术.它使经典亲和色谱原来需要几个小时才能完成的纯化工作缩短为十几分钟或更短,而且纯化倍数高,分离效果好.因此,HPAC在近年基因重组蛋白质的纯化方面得到了广泛的应用.基因重组人白细胞介素-2(rhIL-2)是生物体内具有重要生物学功能的细胞因子,目前已成功地进行了基因表达.本文以自制的rhIL-2单克隆抗体(McAb)的HPAC填料纯化了大肠杆菌(E.coli)表达的rhIL-2.     

High Performance Liquid Affinity Chromatographic Resolution of Trypsins on Soybean Trypsin Inhibitor Bonded Phase

Abstract

An affinity phase was synthesized by immobilizing soybean trypsin inhibitor on epoxysilanized Partisil-10 by direct chemical reaction and resolution of various pancreatic trypsins was studied.     

仿生介孔二氧化硅用于高效液相色谱拆分手性化合物

仿生介孔硅是以有机物作为模板,可有效复刻模板的独特形貌,从而得到其相同或相似结构孔径的介孔硅。本文从仿生的观点出发,从蟹壳中提取得到几丁质膜,将其用作模板制备了仿生手性向列型介孔二氧化硅,并用其制备了液相色谱柱,进行了手性化合物拆分实验。结果表明,该色谱固定相对10个手性化合物有一定的手性分离效果。     

表面引发聚合制备苯乙烯-二乙烯基苯聚合物包覆硅胶固定相

以苯乙烯(St)为单体,二乙烯基苯(DVB)为交联剂,利用表面引发聚合技术制备了聚苯乙烯-二乙烯基苯包覆硅胶固定相.用傅立叶变换红外光谱(FTIR),扫描电子显微镜(SEM),元素分析以及比表面及孔径分析等手段对其性质进行了表征,并以芳环类以及磺胺类化合物为探针,在甲醇/水体系中对其色谱性能进行考察,结果表明该固定相具有较好的反相色谱性能.     

高效液相色谱法所用大孔硅胶填料的制备

对国产ＧＹＱＧ球形硅胶施加高压水热处理并进行扩孔，制备了用于高效液相色谱法的大孔硅胶填料，考察了扩孔压力，扩孔温度和扩孔时间对平均孔径和比表面积的影响。并将产品日本ＳＩＬ－３００３×１０＾－８ｍ硅胶进行了物理性质和孔分布的对比实验，结果表明ＧＹＱＧ硅胶扩孔后平均孔径为２０～３０ｎｍ接近日本ＳＩＬ－３００３×１０＾－８ｍ硅前平平均孔径２５ｎｍ。display structure     

甾醇、甾烷醇柱前衍生高效液相荧光分析

采用荧光衍生化试剂2-(9-咔唑)乙酰氯,对天然产物谷甾醇、豆甾醇、菜油甾醇及谷甾烷醇的柱前衍生化条件,包括催化剂的种类、反应温度、衍生化时间等进行了考察,结果表明催化剂选用三乙胺,反应温度80℃,时间20 min,衍生产物具有恒定的最大检测响应值.利用高效液相色谱对衍生产物进行分析,并对衍生物的分离进行了优化选择,达到了较好的基线分离,检出限为12.6～29.5 nmol/L.方法应用于血清样品的测定,谷甾醇、豆甾醇、菜油甾醇和谷甾烷醇的标准加入回收率分别为101.9%、102.4%、101.0%和103.2%.