高效液相色谱整体柱技术研究进展

高效液相色谱整体柱作为一种新型的分离介质,由于其制备工艺简单、易于修饰改性和分离性能优异,近年来引起了人们的广泛关注。聚合物整体柱具有生物相容性好、柱效高、寿命长、选材范围广、重现性好及使用不受p H限制等优势,广泛应用于食品、化工、农业、环境及生物医学领域小分子化合物及蛋白质的分离和检测,显示出较好的应用前景。本文就近10年液相色谱整体柱的制备、改性方法及应用的研究成果进行综述,并对其在不同应用领域的发展前景作了展望。     

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。     

包覆聚合物高效液相色谱柱填料的研究进展

评述了用于高效液相色谱的包覆聚合物填料的研究进展．该类填料以无机载体为基质，包覆以多种有机聚合物层．这些新型填料既保留了有机聚合物和无机基质的优点，又克服了它们各自的缺陷．包覆的聚合物类型包括聚烃、聚醚、聚酰胺、多糖、多肽、聚硅氧烷、聚胺及多核苷酸等，无机基质包括硅胶、铝胶、钛胶、钻胶及多孔石墨化碳等．包覆聚合物固定相可用于几乎所有色谱方式，如反相高效液相色谱、高效离子交换色谱、手性固定相、超临界流体色谱、体积－排阻色谱，以及亲合色谱．     

聚硅氧烷包夹聚合硅基高效液相色谱固定相的表征及其色谱性能

利用元素分析、红外光谱、扫描电镜及汞压吸附法对制备的聚硅氧烷包夹硅基反相高效液相色谱固定相进行了表征,给出了该固定相的结构信息及其与色谱性能的关系;用滴定法测定了该固定相表面硅羟基数目;考察了该固定相对碱性化合物的分离性能;由表征和色谱性能考察结果可知,该固定相表面的羟基基本被覆盖,因此,可在碱性流动相中长期使用。     

核壳型二氧化硅色谱填料的研究进展

复杂样品的高效快速分离分析是分离科学家所面临的挑战。近年来,核壳型二氧化硅色谱填料以其高效、快速和低背压的特点被广泛用于小分子、大分子和复杂样品的快速分离分析。该文系统综述了二氧化硅核壳色谱固定相快速分离的机理,制备方法及其在小分子、多肽和生物大分子快速分离分析方面的应用,同时对核壳型色谱固定相的发展进行了展望。     

硅胶基质高效液相色谱固定相

结合作者实验室的研究工作,并引用文献157篇,对高效液相色谱用硅胶基质色谱填料进行了综述。     

新型酯型反相高效液相色谱填料的制备,表征及性能评价

将一种新型硅烷偶联剂β－（3，4－环氧环己基）乙基三甲氧基硅烷（β－ECTS）与辛酸反应，然后再键合到硅胶上，得到了酯型键合固定相。用元素分析，^13C固体核磁共振谱，红外光谱进行了表征。以甲醇和水为二元流动相，用包括碱性，酸性和中性有机化合物在内的混合物评价该固定相的疏水性，选择性和亲碱醇基效应，并考察了该填料适用的pH范围及水解稳定性，结果表明，该固定相具有较好的色谱性能，且在pH=2.5-7.5之间稳定性良好，可有效地用于碱性化合物的分析分离。     

全多孔球形硅胶基质高效液相色谱填料研究进展

结合本实验室的研究工作,评述了以全多孔球形硅胶为基质的正相反相色谱填料、手性色谱填料、离子色谱填料以及核一壳型色谱填料的研究进展．     

核苷与碱基的苯胺甲基键合硅胶固定相高效液相色谱分离

建立苯胺甲基键合硅胶固定相(PAMS)高效液相色谱分离核苷与碱基的方法；研究流动相有机溶剂浓度、磷酸缓冲液pH值、离子强度对核苷和碱基在该键合固定相上的色谱保留及分离选择性的影响，用磷酸缓冲液(pH＝4)为流动相快速分离了部分核苷与碱基。     

高效液相色谱蛋白质手性固定性

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。     

离子色谱固定相的发展

 讨论了近年来发展较为活跃的4类离子色谱固定相。共收集文献96篇,其中1995年后发表的文献63篇。 关键词：     

Enthalpy-Entropy Compensation of Octylsilica Stationary Phase in Reversed-Phase HPLC

Abstract

Enthalpy-entropy compensation has been investigated in reversed-phase high performance liquid chromatography with octylsilica stationary phase. The compensation temperatures were determined for this system, and the results show that their change with the composition of the mobile phase was almost similar to that with octadecylsilica stationary phase. It is concluded that the retention mechanism of the separation of alkylbenzenes in both systems with the mobile phase exceed 20% water content is the same.     

纤维状固定相的应用进展

介绍了近年来在固相微萃取、毛细管气相色谱、毛细管电色谱领域出现的一种新型固定相——纤维状固定相。论述了纤维状固定相的类型、特点及应用（引用文献20篇）。     

毛细管电色谱柱及其固定相制备技术的进展

毛细管电色谱结合了毛细管电泳的高分离效率和高效液相色谱的高选择性,因而在这几年受到了越来越多的关注。本文介绍了近期毛细管电色谱柱及其固定相制备方法和应用的进展。     

A Bidenate Amide Bonded Stationary Phase for HPLC

A novel bonded stationary phase, bidenate amide bonded stationary phase (BABSP),was prepared by reacting YWG silica gel firstly with 3-aminopropyltrimethoxysilane, then with diacid chloride. Hydrophobicity, selectivity, and especially silanophilic activity of BABSP were evaluated. The stationary phase exhibited good column efficiency and peak shape for separation of some basic solutes.     

Recent Advances in HPLC Analysis of Analgesics

Abstract

Recent developments in HPLC analysis of analgesics have been rapid, paralleling the growth of chromatographic sciences as a whole. Although analgesics have been used for hundreds of years and chromatgraphic separations have been carried out on them for decades, liquid chromatographic analysis of analgesics has advanced most rapidly in the past 5–7 years . The present review will focus on applications of HPLC to the analysis of commercial analgesics in this time period with emphasis on novel developments and applications associated with the improved accuracy, sensitivity and specificity in herent in current LC systems.     

禾草灵对映异构体在高效液相色谱手性固定相上的拆分

合成了手性纤维素-三(4-甲基苯甲酸酯)(CTMB)，并涂敷于氨丙基硅胶上，制备成手性固定相(CSP)；用高效液相色谱法在该手性固定相上对农药禾草灵外消旋体进行了拆分；考察了流动相组成、温度、醇效应对禾草灵对映体拆分及保留的影响，由实验结果对禾草灵对映体之间的-(ΔG^￠)π,s、（ΔH^￠）π,s、（ΔS^￠）π,s进行了计算，并对其在柱上保留机理进行了讨论。     

Stationary Phases 21: A New Polar Substituted Triazine Stationary Phase for HPLC

A method for preparing a new polar substituted triazine stationary phase is described. The structure of the triazine phase on silica was characterized by elemental analysis, and by FTIR, solid state FT-¹³C NMR, and ²⁹Si NMR spectral analysis. The chromatographic properties of this packing material have been evaluated by using a number of different solutes, and the properties compared with those of a commercial stationary phase RP-18. It is found that this triazine phase has weak π-donor ligands on the silica surface.     

Evaluation of a Doubly Zirconized Silica-Based Stationary Phase for HPLC

This paper describes the preparation, characterization, and application of a chemically bonded and endcapped C18 stationary phase having a doubly zirconized silica support. The stationary phase was characterized using infrared and nuclear magnetic resonance (¹³C and ²⁹Si) spectroscopies, elemental analysis, and surface and thermogravimetric determinations, and evaluated chromatographically using several test mixtures, indicating acceptable efficiency, and asymmetry. The new phase was used for several different applications including the determination of the possible presence of six pesticides in orange juice, using a modified QuEChERS procedure for extraction.

     

Evaluation of a Doubly Zirconized Silica-Based Stationary Phase for HPLC

This paper describes the preparation, characterization, and application of a chemically bonded and endcapped C18 stationary phase having a doubly zirconized silica support. The stationary phase was characterized using infrared and nuclear magnetic resonance (¹³C and ²⁹Si) spectroscopies, elemental analysis, and surface and thermogravimetric determinations, and evaluated chromatographically using several test mixtures, indicating acceptable efficiency, and asymmetry. The new phase was used for several different applications including the determination of the possible presence of six pesticides in orange juice, using a modified QuEChERS procedure for extraction.