高效液相色谱法分离蛋白的大孔硅质固定相的制备及分离机理

介绍了不同孔径的大孔硅胶基质的制备，二醇基和氨基固定相的合成，及其蛋白的分离特性。探讨流动相中的盐浓度和ＰＨ对蛋白保留时间的影响，以及在此两种固定相上蛋白质分离机理的比较。由于大孔填料具有小的比表面积、性容量也低，从而有利于作蛋白质等生物大分子的高效快速分离分析。     

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

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。     

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。     

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。     

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。     

新型纤维素衍生物手性固定相的制备及其对几种对映异构体的高效液相色谱分离

合成了一种经环十二烷修饰的纤维素酯，将其涂敷于小粒径的氨丙基化硅胶（APS）上，制备出高效液相色谱手性固定相，以正己烷、异丙醇为流动相拆分了2-对氯苯基丙腈、1-对氟苯基乙醇、1-对叔丁基苯氧基-2-丙醇、2-对氯苯基辛腈及三唑醇等5种外消旋对映体，并考察了流动相中异丙醇含量对分离效果的影响。     

高效液相色谱质谱质谱法分析人参皂甙

 以反相高效液相色谱法分离了 9种人参皂甙。操作条件为乙腈 水梯度洗脱 ,二极管阵列检测器检测并在2 0 2nm下提取色谱图。利用三级四极杆质谱研究了 9种人参皂甙的一级质谱 (主要给出相对分子质量信息 )和二级质谱 (提供碎片结构信息 )。通过它们质谱图的差异对其进行了鉴别 ,并将方法用于实际样品中的 9种人参皂甙的定性。     

高效液相色谱手性聚合物固定相的研究与进展

对近年来高效液相色谱手性固定相的研究进行了综述。重点介绍了手性聚合物固定相的分类和应用的新进展。讨论了各类手性固定相优缺点,提出了目前存在的问题和今后研究的方向和重点。     

快速高效液相色谱分离技术在中药分析中的应用

中药化学成分分析是中药药效物质阐明及质量控制的关键问题之一。由于中药化学成分的复杂性,中药成分分析一直存在着分离难度大、分析时间长等问题。为此,针对这些问题发展起来的快速、高效液相色谱技术(主要包括超高压液相色谱、基于整体柱的高效液相色谱和高温液相色谱)备受关注。本文结合本实验室近年的研究,对该技术在中药复杂体系化学成分分析中的应用做简要综述,内容主要包括这些技术的原理、分离性能及其在中药复杂体系中的应用。     

高效液相色谱法分离蛋白质的大孔硅质固定相的制备及分离机理

介绍了不同孔径的大孔硅胶基质的制备，二醇基和氨基固定相的合成，及其蛋白质的分离特性。探讨了流动相中的盐浓度和pH对蛋白质保留时间的影响，以及在此两种固定相上蛋白质分离机理的比较。由于大孔填料具有小的比表面积、往容量也低，从而有利于作蛋白质等生物大分子的高效快速分离分析。     

Polysiloxane-encapsulated stationary phase for reversed-phase high-performance liquid chromatography

Summary Silica beads of 6-μm average diameter were silanized with methylvinyldiethoxysilane and then subjected to encapsulation with poly(methylvinylsiloxane). The resulting product is a new stationary phase for reversed-phase high performance liquid chromatography (RP-HPLC) which has superior ability for the separation of polar, non-polar and basic compounds. The chromatographic peaks are symmetric. Its stability has been studied; after continuous use for three months the carbon content and chromatographic behaviour of the phase were unchanged. on to the silica surface to given an uniform organic film. Material prepared in this way has both good chromatographic behaviour and superior selectivity. Because contact of the silica matrix with the mobile phase is avoided, the alkali-resisting ability of the stationary phase is increased. The non-specific adsorption of alkaline solutes on to the silica surface is also avoided because of the complete coverage of surface silanol groups. Reports of stationary phases encapsulated with polystyrene [6], polybutadiene [I] and octadecylsiloxane polymers have recently appeared in the literature [3]. In this paper we report the encapsulation of poly-(methylvinylsiloxane) (analogous to the phase SE-31 often used in GC) on to a silica matrix previously modified with methylvinyldiethoxysilane. The resulting phase has superior performance in reversed-phase HPLC.     

亲水作用色谱固定相及其在中药分离中的应用

亲水作用色谱(HILIC)作为一种分离极性化合物的液相色谱模式,近年来越来越受到关注和重视。一方面是因为强极性化合物的分离问题引起了各个研究领域的重视,如药物分析、代谢组学、蛋白质组学等研究领域都不同程度地涉及强极性化合物的分离问题;另一方面是由于HILIC具有流动相组成简单、分离效率较高、与质谱兼容以及反压较低等优势。固定相是HILIC发展和应用的基础,本文主要从固定相分子结构的角度对HILIC固定相的结构特征、保留特性以及应用概况等进行了综述。对传统正相色谱固定相用于HILIC以及专门设计的HILIC固定相进行了介绍,评述了各自的优缺点和应用概况;对近年来HILIC固定相在中药分离中的应用进行了介绍;并对HILIC固定相的发展进行了展望。     

Cholesteric bonded stationary phases for high-performance liquid chromatography: a comparative study of the chromatographic behavior

The properties of four cholesteric bonded stationary phases differing in the nature of the spacer and the end-capping were assessed using simple chromatographic tests based on the retention of nonpolar compounds and of planar or nonplanar probe solutes. All cholesteric columns showed a hydrophobicity close to that of conventional octadecyldimethylsilyl (ODS) materials. Non-end-capped cholesteric bonded phases showed greater selectivity than ODS ones and both end-capped cholesteric bonded phases exhibit behavior intermediate between that of the non-end-capped original material and that of the ODS bonded phase.     

Computer-assisted transposition of conditions in high-performance thin-layer chromatography to high-performance liquid chromatography for the separation of pesticides

Summary A computer-assisted method is presented for mobile phase selection for the optimal separation of pesticides by HPTLC and HPLC. The system is based on a plot of solute retention value and separation criterion vs. binary mobile phase composition for graphic optimization. The result of HPTLC can be transposed to HPLC for optimal separation. The transposition equation is given.     

Per(3-chloro-4-methyl)phenylcarbamate cyclodextrin clicked stationary phase for chiral separation in multiple modes high-performance liquid chromatography

In this work, a detail study has been performed on the enantioselectivity of per(3-chloro-4-methyl)phenylcarbamate-β-CD clicked chiral stationary phase (CSP) in high-performance liquid chromatography. Both normal phase and polar organic mobile phases have been explored for the enantioseparation of 39 model racemic pairs including aromatic alcohols, flavonoids, β-blockers and amino acids. Chiral resolution values over 10 were achieved for flavonoids. The comparison study with reference perphenylcarbamate-β-CD clicked CSP reveals the significance of 3-chloro-4-methyl functionality in improving the enantioselectivities. This study may provide insight on the multiple interactions between functionalized CD and analytes.     

Retention mechanism divergence of a mixed mode stationary phase for high performance liquid chromatography

Mixed mode stationary phases utilize secondary retention mechanisms to add a dimensionality to the surface of high performance liquid chromatography (HPLC) adsorbents. This approach was used by several authors to improve the separation performance of single dimension separations. We explored the magnitude of these secondary interactions by performing an off-line two-dimensional (2D)-HPLC separation with a Scherzo SM-C18 column of a β-lactoglobulin tryptic digest with a mobile phase pH of 7 in the first dimension and 2 in the second. Mechanism divergence was determined using the peak capacity and a geometric approach to factor analysis, to measure the correlation. This separation was repeated with a C18 stationary phase as a control. It was found that the C18 column had a correlation coefficient of 0.784, smaller than the mixed mode column, 0.884. This indicated that the retention mechanisms of the C18 column were more divergent under these two pH environments than the mixed mode column. However, the SM-C18 still provided alternative selectivity of the peptides to that of the C18 and could be considered as a good alternative for further 2D-HPLC separations.     

Porous glassy carbon,a new columns packing material for gas chromatography and high-performance liquid chromatography

Summary A new carbon for liquid and gas chromatography, called porous glassy carbon (PGC) is described. The material is made using a porous template filled with carbonizable resin. After firing in an inert atmosphere the template is removed. PGC has been made with surface area ranging from 20 m²/g to 400 m²/g. It is of adequate strength for gas and high-performance liquid chromatography. In gas chromatography it is similar to the commerical graphitized thermal carbon black (GTCB) Carbopack B, but has somewhat less retention per unit surface area and is much more robust. It gives symmetrical peaks for hydrocarbons with k-values up to at least 100. In liquid chromatography it is similar to the GTCB's coated with pyrolytic carbon described by Guiochon. It behaves as a strong reversed phase adsorbent. Fairly good peak symmetry is maintained for k-values up to at least 10 but trace additives to the eluent may be necessary to control peak asymmetry. PGC has considerable potential as a new packing material in both gas and liquid chromatography.Presented at the 14th International Symposium on Chromatography London, September, 1982     

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.     

Covalently bonded polysaccharide-modified stationary phase for per aqueous liquid chromatography and hydrophilic interaction chromatography

The mixed sulfated/methacryloyl polysaccharide derivative was prepared and successfully immobilized onto the surface of porous silica particles by polymerization. Polysaccharide derivative was calculated as 10.33% in the stationary phase prepared. The new stationary phase (PMSP) showed both hydrophilic interaction (HILIC) and per aqueous liquid chromatography (PALC) characteristics. The effects of column temperature, the water content, pH and ion strength of mobile phase on the retention time of test compounds in highly aqueous eluents were investigated to evaluate the PALC features of PMSP. The column efficiency is about 31,000 plates/m for benzoic acid in water/ACN (97/3, v/v) mobile phase at a flow rate of 1.0 mL/min. Compared with C18 column, the PMSP had shorter retention time for weak polar and non-polar compounds, but also showed stronger retention for strong polar compounds. It indicated that PALC was a suitable mode of chromatography as replacement of HILIC and complementarity of reversed-phase liquid chromatography (RPLC).