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。     

咪唑键合硅胶液相色谱固定相的反相色谱行为

采用嫁接法制备了一种新型高效液相色谱固定相.考察了固定相的液相色谱保留行为,发现该键合相具有很强的阴离子交换作用,还同时存在反相疏水作用.利用其疏水作用,可以对一些简单的有机化合物进行分离.     

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。     

咪唑键合硅胶液相色谱固定相的正相色谱行为

该文将咪唑键合硅胶液相色谱固定相填充到毛细管中,在自制的微柱液相色谱系统下以碱性(胺类)和酸性(酚类)化合物为溶质对该固定相的正相色谱行为进行考察.结果表明该键合相在正相色谱模式下对碱性化合物具有良好的分离选择性,而酸性化合物在流动相中加入改性剂乙酸的条件下也实现了较好的分离.研究表明,正相模式下该键合相的保留机理存在着氢键、静电吸引及π-π等相互作用机制.     

新型吡咯烷键合反相高效液相色谱固定相的制备与研究（英文）

正A new ionic liquid-based high-performance liquid chromatography stationary phase is reported.A derivative of N-methyl pyrrolidinium tetrafluoroborate was covalently immobilized on the surface of silica particles to prepare silica-based N-methyl pyrrolidinium tetrafluoroborate(SilprMP BF4)stationary phase.The obtained ionic liquid-modified silica was evaluated and confirmed by elemental analysis,infrared spectroscopy,and thermogravimetric analysis.A column was packed with the modified particles.The retention behavior of aromatic compounds,alkyl benzenes,and acidic and basic compounds on the SilprMP BF4 stationary phase was studied under reversed-phase liquid chromatography conditions.The effect of the eluent pH on the separation of the acidic and basic compounds was also studied.The new stationary phase involves multiple retention mechanisms,such as electrostatic,hydrophobic,ion-dipole,and anion-exchange interactions,which might lead to multipurpose separation media.     

高效液相色谱氮杂冠醚键合固定相的合成及性能研究

我们曾用γ－氯丙基键合硅胶（ＣＰＳ），在氢化钠（ＮａＨ）作用下合成了３－（氮杂－１８－冠－６）丙基键合固定相（ＢＣＰ）［１］．该固定相对碱基、核苷酸、硝基苯酚等有较好的分离选择性，但由于ＮａＨ对硅胶基质腐蚀作用较大，导致ＢＣＰ柱效及渗透性较低．本文采...     

新型高效液相色谱酰胺键合固定相的制备与评价

将YWG-80硅胶和3-氨基丙基三甲氧基硅烷反应后与2-壬基丁二酰氯反应制得一种新型双齿酰胺键合固定相(BABSP-2)。采用元素分析和傅里叶变换红外光谱表征了键合相;用芳香族化合物溶质和甲醇-水二元流动相,考察了键合相的疏水选择性和亲硅醇基活性;评估了在酸性条件下(pH2.5)的水解稳定性。结果表明：BABSP-2能有效抑制残留硅醇基活性,并具有可比的疏水选择性和较好的水解稳定性。     

一种新型液相色谱屏蔽键合相的色谱性能

烷基硅胶键合固定相 ,特别是十八烷基键合固定相 ,是应用最广泛的反相色谱固定相 ,改变流动相组成 ,就可实现大多数有机化合物的分离分析 .但是 ,由于硅胶表面残留硅醇基的存在 ,分离某些极性化合物 ,特别是碱性有机化合物时使色谱峰变形拖尾 ,灵敏度下降 .采用封端技术也不能完全消除残留硅醇基的影响 .在分离碱性物质时大都采用缓冲溶液流动相 ,长期使用缓冲溶液将影响仪器和色谱柱的性能和寿命 .近年来 ,为了改善碱性化合物的分离 ,提出了空间保护相 [1] 和烷基酰胺屏蔽相 [2 ,3] .依据静电屏蔽原理 ,我们 [4 ]曾制备了十四烷基胺反相色…     

桥联β-环糊精液相色谱键合固定相研究

合成了两种桥联β-环糊精固定相,将其用于芳香烃位置异构体、氨基酸的对映异构体的拆分,同时比较了其与β-CD固定相的手性拆分效果。研究结果表明,桥联环糊精固定相对一些对映异构体具有较好的选择性;其对普通的环糊精固定相的选择性具有一定的补充或者改进作用。     

姜黄素键合硅胶固定相高效液相色谱分离取代芳香酸类化合物

研究了13种取代芳香酸类化合物在姜黄素键合硅胶固定相(CCSP)上的色谱行为,考察了甲醇含量、流动相pH值对CCSP分离取代芳香酸类化合物的影响,探讨了该固定相对芳香酸类化合物的色谱保留机理,并应用于实际样品复方水杨酸搽剂的分离分析。结果表明,在不同含量的甲醇-0.02 mol.L-1NaH2PO4(pH=2.5)流动相体系中,三组芳香酸标准混合样和实际样品中四种主要成分在CCSP上实现基线分离。与ODS柱相比,在相同条件下,CCSP对这类酸性化合物具有较高的选择性,且对13种取代芳香酸类化合物的洗脱顺序与ODS具有显著差异,其中5种溶质在CCSP上的保留强于ODS,这说明不同保留机理的存在。研究表明,CCSP具有典型的反相色谱特征,但疏水性较ODS弱;除疏水作用外,n-π和π-π作用、氢键作用、电荷转移作用、偶极-偶极作用对分离也有贡献。CCSP对极性、电离性物质如水杨酸、对硝基苯甲酸、3,4,5-三羟基苯甲酸、邻苯二甲酸和邻溴苯甲酸等具有较强的保留;由于CCSP较弱的疏水性和多种分离机制,邻氯苯甲酸和苯甲酸在CCSP上的保留不会像在ODS上那么强,且分离度明显优于ODS。     

New Stationary Phase Prepared by Immobilization of a Copper-Amine Complex on Silica and Its Use for High Performance Liquid Chromatography

Chromatographic silica (10 μm) was chemically modified with the silylating agent: [3-(2-aminoethyl)aminopropyl]trimethoxysilane (AEAPTS). The reaction product was characterized by elemental analysis and infrared and ¹³C and ²⁹Si NMR spectra. The chemically modified silica was treated with Cu(II) in methanol medium. This cation was strongly adsorbed through complexation by the pendant ethylenediamine groups attached to the silica surface. The complex formed on the silica surface was shown to be stable in both aqueous and non-aqueous media. The aim of Cu(II) immobilization is to use this new material as a stationary phase in High Performance Liquid Chromatography (HPLC). Separations of synthetic mixtures of aromatic amines and of polyaromatic hydrocarbons were undertaken using 150×3.9 mm HPLC columns packed with the modified silica, with and without copper ions, to follow the influence of the cation on the chromatographic separation and to verify the efficiency of the new stationary phase for HPLC.     

A New Definition of the Stationary Phase Volume in Mixed-Mode Chromatographic Columns in Hydrophilic Liquid Chromatography

Polar columns used in the HILIC (Hydrophilic Interaction Liquid Chromatography) systems take up water from the mixed aqueous–organic mobile phases in excess of the water concentration in the bulk mobile phase. The adsorbed water forms a diffuse layer, which becomes a part of the HILIC stationary phase and plays dominant role in the retention of polar compounds. It is difficult to fix the exact boundary between the diffuse stationary and the bulk mobile phase, hence determining the column hold-up volume is subject to errors. Adopting a convention that presumes that the volume of the adsorbed water can be understood as the column stationary phase volume enables unambiguous determination of the volumes of the stationary and of the mobile phases in the column, which is necessary for obtaining thermodynamically correct chromatographic data in HILIC systems. The volume of the aqueous stationary phase, Vex, can be determined experimentally by frontal analysis combined with Karl Fischer titration method, yielding isotherms of water adsorbed on polar columns, which allow direct prediction of the effects of the composition of aqueous–organic mobile phase on the retention in HILIC systems, and more accurate determination of phase volumes in columns and consistent retention data for any mobile phase composition. The n phase volume ratios of 18 columns calculated according to the new phase convention strongly depend on the type of the polar column. Zwitterionic and TSK gel amide and amine columns show especially strong water adsorption.     

新型离子交换硅胶键合相的制备及评价

二甲基氯硅烷与硅胶表面反应,形成牢固的ＳｉＨ键之后,连接上活泼的中间体——烯丙基缩甘油醚作为柔软的分子臂,最后接上二乙基氨基,由此制得了新型的离子交换硅胶键合相。经漫反射红外光谱、元素分析和高效液相色谱法对键合相进行了鉴定和评价。结果表明：键合反应按预定路线进行,键合相具有较好的色谱性能。此种方法可有效地运用于无孔硅胶填料的制备。     

Preparation and Characterization of a New Quercetin‐bonded Stationary Phase for High Performance Liquid Chromatography

A quercetin‐bonded silica gel stationary phase (QUSP) containing natural flavonoid ligand was first prepared via γ‐glycidoxypropyltrimethoxysilane (KH‐560) as a coupling reagent for high‐performance liquid chromatography. Its chemical structure was characterized by Fourier infrared spectroscopy, elemental analysis, thermal thermogravimetry and ¹³C cross polarization/magic angle spinning nuclear magnetic resonance (CP/MAS NMR). The chromatographic property of QUSP was systematically evaluated by using neutral, basic and acidic aromatic compounds as probes. In order to clarify its retention mechanism, a comparative study of QUSP with conventional octadecylsilyl‐bonded stationary phase (ODS) was also carried out under the same conditions. The results showed that the new quercetin‐bonded phase exhibited an excellent reversed‐phase chromatographic property with relatively weak hydrophobicity. However, it has an advantage over ODS in the fast separation of polar aromatic compounds because the quercetin ligand could provide various sites besides hydrophobicity, such as hydrogen bonding, dipole‐dipole, π‐π staking and charge transfer interactions. QUSP was performed in the baseline separations of ionized polar basic or acidic compounds, including pyridines, anilines, pyrimidines, purines and phenols with symmetric peak shape in common mobile phases without buffer salt within relatively short time. The natural ligands from herbs are readily available and contain a variety of active sites, which facilitate the exploration of industrial chromatographic separation materials for green products.     

一种新的改性聚乙二醇毛细管气相色谱固定相

合成了一种新的聚乙二醇衍生物，将其用作毛细管气相色谱固定相，研究了其色谱性能，并成功地分离了二甲苯、氯甲苯、溴甲苯、二氯苯等二取代苯位置异构体；并对其手性分离能力进行了初步研究和讨论。     

聚硅氧烷键合的离子液体用作高温气相色谱固定相的研究

合成了阴离子为二(三氟甲基磺酸酰)亚胺(NTf-2)的新型聚硅氧烷键合离子液体 ([PSOMIm][NTf2]),并采用静态涂渍法,制备了毛细管气相色谱柱.该固定相具有良好的热稳定性.热重测试显示,温度高于380 ℃后,[PSOMIm][NTf2]开始缓慢分解.色谱性能评价显示,此固定相对多种异构体和同系物均具有良好的分离选择性和高的热稳定性.对Grob试剂的分离结果表明,各种组分均能在柱上得到良好的分离且峰的对称性很好.此新型聚合物离子液体在高温气相色谱固定相的研究和应用方面具有较大的潜力.     

高效液相色谱中的纤维素衍生物手性固定相

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。     

高效液相色谱蛋白质手性固定相

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。     

聚合物涂敷反相高效液相色谱固定相

对聚合物涂敷反相高效液相色谱固定相的制备及其特性进行了综述。根据制备方法对固定相进行了分类,并指出该类固定相对色谱峰拖尾现象的改善引人注目,且就涂敷物对基质孔径及色谱性能的影响进行了讨论。另外,对该类固定相的稳定性进行了阐述。