近几年国内外离子液体气相色谱柱的进展

室温离子液体由于它具有十分特殊的性质,得到了各个领域广泛的应用,近几年在气相色谱中应用室温离子液体作固定相的研究成为气相色谱的热点,这主要是由于新开发出来的离子液体可以很好地满足气相色谱固定相的要求。对近几年室温离子液体在气相色谱中的应用做一简要综述。     

气相色谱固定相的演变

简要综述了半个世纪以来气相色谱固定相的发展,在气相色谱发展的初期主要是低分子化合物和工业用高聚物,主要用于填充柱气相色谱,有上千种固定液。到上世纪80年代以后毛细管柱气相色谱起主导作用,固定液数量减少、质量提高,最常用的有五六种。到上世纪90年代以后固定相的研究以手性固定相和提高常规固定相的性能为主。进入21世纪,各个制备色谱柱的公司不断推出高性能、低流失、重复性好和专用型毛细管柱色谱柱,以适应研究和实际需要。     

超临界CO2色谱拆分手性农药的研究进展

综述了国内外超临界CO2色谱拆分手性农药的研究进展,概述了超临界CO2技术的优越性以及色谱的手性固定相、流动相和操作条件,并介绍了制备型超临界CO2色谱的应用.     

凹凸棒石粘土的分离性能及其在离子色谱固定相研究中的应用前景

凹凸棒石粘土具有独特的空间结构和较大的比表面积,具有较强的离子交换性质和吸附性质,应用广泛。其对金属离子和有机污染物的吸附研究报道较多。利用其对不同组分的吸附作用的差异和选择合适的流动相,凹凸棒石粘土可用作离子色谱固定相。本文总结了凹凸棒石粘土对金属离子和有机污染物的吸附作用研究,分析了其作为离子色谱固定相的巨大潜力。     

硫酸铬钾结晶水合物用作气相色谱固定相的研究

硫酸铬钾结晶水合物用作气相色谱固定相的特性进行了研究 ,结果表明 ,其色谱性能良好 ,可作固定相使用。     

金属有机骨架材料在开管毛细管电色谱中的应用

开管毛细管电色谱通过电泳和色谱效应进行化学分析。近年来应用方面的研究多为将高选择性固定相引入毛细管的内表面进行不同化合物的分离分析。金属有机骨架材料是重要的固定相之一。对开管毛细管电色谱的MOFs涂层材料,涂层方法,分离机理,分离物质进行了简单综述。其应用对医药,农业,食品工业都具有重要的参考价值。     

金属丝网载体气液色谱分离过程的研究

采用金属丝网填料作为固定相的载体,构建了制备气液色谱装置,并采用提前气化这种新进样方式。通过对二元共沸物正丙醇-水的分离考察了所构建制备气液色谱装置的分离过程。实验结果表明,采用金属丝网填料作为制备气液色谱固定相的载体是完全可行的;提前气化进样方式具有易于实现大进样量的优点。     

基于SI—ATRP技术制备接枝聚乙烯基四唑色谱固定相及性能研究

应用表面引发原子转移自由基聚合技术（SI—ATRP）,以合成的功能单体乙烯基四唑（VT）为单体,以自制的6．0μm单分散大孔交联聚甲基丙烯酸环氧丙酯（PGMA／EDMA）微球为基质,合成了新型弱阳离子交换并具有亲水作用的色谱固定相填料。控制VT单体与引发剂的比率,得到了接枝密度和链长可控的接枝聚乙烯基四唑（PVT）固定相。并考察了聚合反应过程,单体的合成与表征,弱阳离子交换性能、亲水性能等方面。实验结果表明,该色谱固定相色谱性能良好。     

高效液相色谱手性固定相在药物分析中的应用

高效液相色谱(HPLC)手性固定相是手性色谱发展的关键,应用手性固定相对药物对映体的拆分在药物工业中起着重要的作用。综述了高效液相色谱几种主要手性固定相的特性,并重点对其中4种手性固定相在药物分析中的应用作了介绍。     

直接气相色谱法测定苹果酸,富马酸中的顺丁烯二酸

提出了一种直接气化进样分析苹果酸,富马酸中顺丁烯二酸含量的色谱方法,使用SF-96固定相,柱温150℃。探讨了顺丁烯二酸在该固定相上的色谱行为。方法的回收率为97％～99％,变异系数2.0％～4.5％。     

[CHTA+][Tf2N-]离子液体作为气相色谱新型固定相的性能研究

合成了一种手性离子液体[ CHTA+][Tf2N-]((S)-(-)-(3-氯-2-羟丙基)三甲基铵双三氟甲烷磺酰亚胺),将其用作新型气相色谱固定相,考察了它的色谱性能.研究结果表明:该离子液体作为气相色谱固定相在容量因子为1.29时,其理论塔板数为2 057块/米；对醇类、酮类、芳香族化合物、位置异构体以及一些外消旋体具有良好的分离效果.     

2,5-二甲基-3,4-二苯基苯基接枝聚硅氧烷气相色谱固定相

合成了2,5-二甲基-3,4-二苯基苯基接枝聚硅氧烷气相色谱固定相,接枝量分别为10％、20％、30％,静态法涂柱,评价了其色谱性能.该类固定相柱效高、使用温度范围宽、热稳定性好,适用于芳烃混合物、苯类取代物、稠环芳烃化合物的分离分析.     

离子液体在色谱分析中的应用

综述了近年来国内外离子液体在色谱分析中的应用情况,主要包括离子液体用作气相色谱固定相,液相色谱流动相或流动相添加剂,以及毛细管电泳电解质、添加剂或涂布于毛细管壁上分离各种物质。     

离子液体作为气相色谱固定相的参数测定

将疏水性离子液体[BMIM]PF6用于气相色谱固定相中,检测分离环己烷、甲苯、邻二甲苯混合有机溶剂,并与邻苯二甲酸二壬酯填充柱对这3种物质的分离效果进行比较。实验结果表明：邻苯二甲酸二壬酯柱虽然也能将这3种物质分开,但各物质出峰太慢、保留时间长、峰高太低,而疏水性离子液体[BMIM]PF6柱对这3种物质有很好的分离效果,各物质保留时间缩短、峰高增强,由此得出离子液体作为气相色谱固定相对分离这类有机物的优势。     

Analytical Methods for Determination of Polycyclic Aromatic Hydrocarbons (PAHs) — A Historical Perspective on the 16 U.S. EPA Priority Pollutant PAHs

The identification of 16 polycyclic aromatic hydrocarbons (PAHs) as priority pollutants by the U.S. Environmental Protection Agency (EPA) in 1976 has been a primary driver for analytical methods development for the determination of PAHs. In this article, the historical development of methods in liquid chromatography (LC) and gas chromatography (GC) to separate these 16 PAHs is discussed. In LC a significant effort was the search for and the fundamental understanding of the unique stationary phase capable of achieving the desired separation of the 16 EPA PAHs. For GC methods, the focus on stationary phase development has been the separation of critical isomers with a broader scope than the 16 EPA PAHs. The current routine LC and GC methods for the 16 EPA PAHs are well established; however, new advances in analytical techniques beyond LC and GC are discussed. Many analysts are now interested in more than just the 16 EPA PAHs (e.g., higher molecular mass PAHs and alkyl-substituted PAHs) and analytical methods have emerged to address these needs. Reference materials and their use in the determination of PAHs are discussed.     

聚乙二醇600油酸酯作为气相色谱固定液的研究与应用

本文用聚乙二醇600和油酸合成了聚乙二醇600油酸酯非离子型表面活性剂，精制后作为气相色谱固定液，制备成色谱柱。测定此固定液的最高使用温度、相对极性。对一些混合物组分的分离效果表明了此固定液具有良好的应用性能，是一种新型的气相色谱固定液。     

Chromatographic Evaluation of Octadecyl-Bonded SiO2/SiO2-Based Stationary Phase for Reversed-Phase High Performance Liquid Chromatography

A new type of octadecyl-bonded SiO₂/SiO₂ (ODSS) core–shell monodisperse silica spheres was prepared as a high performance liquid chromatography stationary phase. The chromatographic performance was evaluated and compared with totally porous octadecyl-bonded SiO₂. Various methods were used for characterization of the two column packings for reversed-phase chromatography in terms of permeability, hydrophobic selectivity, sensitivity, stability and hydrophobicity. The results showed that the ODSS-based stationary phase has enhanced permeability, good hydrophobic selectivity, high chemical stability and sensitivity. Acidic, basic and neutral aromatic compounds were separated on the two types of stationary phases. The ODSS-based stationary phase has good selectivity and gives symmetrical narrow peaks under reversed-phase conditions.     

毛细管气相色谱柱近年的发展

简要地阐述了近几年毛细管气相色谱柱的发展和特点.GC的色谱柱制柱工艺是一个成熟的技术,所以在制柱工艺方面的研究不够活跃.近年新研究的固定相集中在常温离子液体和各种环糊精的衍生物.20世纪GC毛细管色谱柱柱工艺的研究主要在研究机构和学校中进行,而近几年GC毛细管色谱柱的研究和改进集中在色谱柱厂家进行,并立即成为商品柱.近年GC分析所用的色谱柱大都使用毛细管柱,并趋向于使用商品GC毛细管柱,所使用的商品色谱柱中,最多的是以含5%苯基的聚甲基硅氧烷色谱柱.     

Application of Ionic Liquids in High Performance Reversed-Phase Chromatography

Ionic liquids, considered “green” chemicals, are widely used in many areas of analytical chemistry due to their unique properties. Recently, ionic liquids have been used as a kind of novel additive in separation and combined with silica to synthesize new stationary phase as separation media. This review will focus on the properties and mechanisms of ionic liquids and their potential applications as mobile phase modifier and surface-bonded stationary phase in reversed-phase high performance liquid chromatography (RP-HPLC). Ionic liquids demonstrate advantages and potential in chromatographic field.     

Metal-organic frameworks for analytical chemistry: from sample collection to chromatographic separation

In modern analytical chemistry researchers pursue novel materials to meet analytical challenges such as improvements in sensitivity, selectivity, and detection limit. Metal-organic frameworks (MOFs) are an emerging class of microporous materials, and their unusual properties such as high surface area, good thermal stability, uniform structured nanoscale cavities, and the availability of in-pore functionality and outer-surface modification are attractive for diverse analytical applications. This Account summarizes our research on the analytical applications of MOFs ranging from sampling to chromatographic separation. MOFs have been either directly used or engineered to meet the demands of various analytical applications. Bulk MOFs with microsized crystals are convenient sorbents for direct application to in-field sampling and solid-phase extraction. Quartz tubes packed with MOF-5 have shown excellent stability, adsorption efficiency, and reproducibility for in-field sampling and trapping of atmospheric formaldehyde. The 2D copper(II) isonicotinate packed microcolumn has demonstrated large enhancement factors and good shape- and size-selectivity when applied to on-line solid-phase extraction of polycyclic aromatic hydrocarbons in water samples. We have explored the molecular sieving effect of MOFs for the efficient enrichment of peptides with simultaneous exclusion of proteins from biological fluids. These results show promise for the future of MOFs in peptidomics research. Moreover, nanosized MOFs and engineered thin films of MOFs are promising materials as novel coatings for solid-phase microextraction. We have developed an in situ hydrothermal growth approach to fabricate thin films of MOF-199 on etched stainless steel wire for solid-phase microextraction of volatile benzene homologues with large enhancement factors and wide linearity. Their high thermal stability and easy-to-engineer nanocrystals make MOFs attractive as new stationary phases to fabricate MOF-coated capillaries for high-resolution gas chromatography (GC). We have explored a dynamic coating approach to fabricate a MOF-coated capillary for the GC separation of important raw chemicals and persistent organic pollutants with high resolution and excellent selectivity. We have combined a MOF-coated fiber for solid-phase microextraction with a MOF-coated capillary for GC separation, which provides an effective MOF-based tandem molecular sieve platform for selective microextraction and high-resolution GC separation of target analytes in complex samples. Microsized MOFs with good solvent stability are attractive stationary phases for high-performance liquid chromatography (HPLC). These materials have shown high resolution and good selectivity and reproducibility in both the normal-phase HPLC separation of fullerenes and substituted aromatics on MIL-101 packed columns and position isomers on a MIL-53(Al) packed column and the reversed-phase HPLC separation of a wide range of analytes from nonpolar to polar and acidic to basic solutes. Despite the above achievements, further exploration of MOFs in analytical chemistry is needed. Especially, analytical application-oriented engineering of MOFs is imperative for specific applications.