开管毛细管色谱柱的制备及其在蛋白质组学研究中的应用进展

近年来随着生命科学等领域的深入发展,人们对微量样本分离分析的需求越来越高,液相色谱系统的微量化受到了更多的关注。由于开管毛细管色谱柱具有较低的反向压力,可通过采用更长的色谱柱提高柱效,从而实现对复杂生物样本的高效分离,因而成为液相色谱柱新的发展方向。本文对开管毛细管色谱柱的制备方法及应用进展进行了综述。     

溶胶-凝胶法制备毛细管硅胶整体柱的研究进展

毛细管硅胶整体柱作为一种新型的分离介质,在色谱领域显示出了强大的生命力。本评述介绍了溶胶-凝胶法制备毛细管硅胶整体柱的方法,重点分析了溶胶-凝胶法制备毛细管硅胶整体柱的影响因素,总结了近几年毛细管硅胶整体柱在高效液相色谱和电色谱中的应用。     

Persilylation of glass capillary columns. Part 4: Discussion of parameters

Persilylated glass capillary columns are the most universal GC columns available. They are relatively easy to prepare, but there is nevertheless a great need for helpful practical instructions. In the recent literature, methods and conditions for the preparation of persilylated columns have been recommended, but these might confuse the individual column maker, since they seem to originate from limited observations rather than from comprehensive investigation. They will hardly help to make column preparation safer. This paper attempts a summarized view of the present experience with persilylation and provides basic information for column makers.     

窄内径多孔层开管柱的制备及在液相色谱中的应用

近年来,微纳分离技术由于其内在的优势而受到越来越多的关注.多孔层开管柱是一种重要的微分离柱形式,与粗内径的多孔层开管柱(>25μm)相比,窄内径的多孔层开管柱具有更高的分离效率和更低的试剂消耗量.本文综述了内径≤25μm的窄内径多孔层开管毛细管柱的制备方法、与质谱检测联用技术以及在液相色谱中的应用研究进展,对其发展前景进行了展望.     

毛细管离子色谱进展

从毛细管离子色谱柱制备和毛细管离子色谱仪器研制两方面评述了毛细管离子色谱目前的发展状况。毛细管离子色谱柱包括开管离子色谱柱，毛细管颗粒填充离子色谱柱以及最近几年发展起来的整体毛细管离子色谱柱。对毛细管离子色谱仪的总结包括微流量泵、小体积进样器、适合毛细管离子色谱系统的小体积抑制器、电导和光学检测器等。     

Preparation and use of packed capillary columns in chromatographic and related techniques

In this paper general considerations related to the various approaches and parameters influencing the preparation of highly efficient and stable capillary columns for use in liquid chromatography and related techniques are presented and the column production process is discussed in some detail. The different packing methods available for delivering a packing material into a capillary column are discussed from a practical viewpoint. Packing with a gas (dry packing), packing with a liquid solvent or a mixture of solvents (slurry packing), packing with supercritical carbon dioxide, electrokinetic packing, and sol-gel packing technologies are introduced and discussed throughout the paper. Practical recommendations for obtaining highly efficient (high plate numbers) and stable capillary packed columns are also addressed and discussed.     

Preparation of High Performance Alumina PLOT Columns and Analysis of Light Hydrocarbons

With the introduction of new capillary column coating technique.It has been realized to prepare gas chromatograph of very high resolution. There has been continued interest in extending the use of GSC adsorbent to capillary chromatography. Currently the film built up on the inner surface of the capillary column can be quite homogeneous and the separation efficiency of the column is increased as well. There have been numerous papers that describe the preparation of PLOT columns in detail. However, Owing to the complexity of the preparation of porous layer for capillary GSC. It is still urgently need to extensively study the preparation process in order to get desired capillary columns of high quality and good reproducibility. This paper describe a new coating method of high performance PLOT columns with alumina by means of liquid phase deposition other than dynamic or static coating techniques. The selectivity, reproducibility and separation power of the column in analysis of light hydrocarbons were examined.     

Monolithic column in gas chromatography

Monolithic columns invented in chromatographic praxis almost 40 years ago gained nowadays a lot of popularity in separations by liquid chromatographic technique. At the same time, application of monolithic columns in gas chromatography is less common and only a single review published by Svec et al. [1] covers this field of research. Since that time a lot of new findings on application and properties of monolithic columns in gas chromatography have been published in the literature deserving consideration and discussion. This review considers preparation of monolithic columns for GC, an impact of preparation conditions on column performance, optimization of separation conditions for GC analysis on monolithic columns and other important aspects of preparation and usage of monolithic capillary columns in GC. A final part of the review discusses the modern trends and possible applications in the future of capillary monolithic columns in GC.     

Porous structure of the monolithic sorbent and separation properties of monolithic capillary columns in gas and liquid chromatography

Macroporous polymer based on polydivinylbenzene was used for the preparation of monolithic capillary columns with the diameter from 0.01 to 0.53 mm for separations by gas and liquid chromatography. The separation properties of the columns were studied by analysis of model systems of aromatic (in liquid chromatography) and light (in gas chromatography) hydrocarbons. The permeability was determined and the C parameter of the Van-Deemter equation was found for each column. The permeability of the majority of columns determined by gas chromatography is independent of the column diameter. The permeability of the same columns in liquid chromatography is also almost constant for the columns 0.53–0.1 mm in diameter; however, the permeability decreases sharply on going to columns of smaller diameter. In gas chromatography the value of the C parameter reflecting the effect of the mass transfer of the sorbate between the mobile and stationary phases on the smearing of a chromatographic peak in the column approximately the same for all columns. In liquid chromatography the value of the C coefficient in the Van-Deemter equation for the same capillary columns changes with a change in the column diameter and reaches a minimum for the columns 0.1 mm in diameter. The differences observed for the characteristics of the columns in gas and liquid chromatography are due to different structures of the macroporous monolith formed in columns of different diameter and to the effect of solvation of the monolith by the mobile phase under the conditions of liquid chromatography.     

溶胶-凝胶法制备开管毛细管柱的研究进展

介绍了溶胶-凝胶法制备开管毛细管柱的方法,分析了溶胶-凝胶法制备开管毛细管柱的影响因素和特点,总结了溶胶-凝胶技术在毛细管气相色谱柱、毛细管液相色谱柱、毛细管电泳柱及电色谱柱方面的应用进展。     

Polymethacrylate monolithic columns for capillary liquid chromatography

In recent years, continuous separation media have attracted considerable attention because of the advantages they offer over packed columns. This research resulted in two useful monolithic material types, the first based on modified silica gel and the second on organic polymers. This work attempts to review advances in the development, characterization, and applications of monolithic columns based on synthetic polymers in capillary chromatography, with the main focus on monolithic beds prepared from methacrylate-ester based monomers. The polymerization conditions used in the production of polymethacrylate monolithic capillary columns are surveyed, with attention being paid to the concentrations of monomers, porogen solvents, and polymerization initiators as the system variables used to control the porous and hydrodynamic properties of the monolithic media. The simplicity of their preparation as well as the possibilities of controlling of their porous properties and surface chemistries are the main benefits of the polymer monolithic capillary columns in comparison to capillary columns packed with particulate materials. The application areas considered in this review concern mainly separations in reversed-phase chromatography, ion-exchange chromatography, hydrophobic and hydrophilic interaction modes; enzyme immobilization and sample preparation in the capillary chromatography format are also addressed.     

Automated sample preparation using in-tube solid-phase microextraction and its application -- a review

Sample preparation, such as extraction, concentration, and isolation of analytes, greatly influences their reliable and accurate analysis. In-tube solid-phase microextraction (SPME) is a new effective sample preparation technique using an open tubular fused-silica capillary column as an extraction device. Organic compounds in aqueous samples are directly extracted and concentrated into the stationary phase of capillary columns by repeated draw/eject cycles of sample solution, and they can be directly transferred to the liquid chromatographic column. In-tube SPME is an ideal sample preparation technique because it is fast to operate, easy to automate, solvent-free, and inexpensive. On-line in-tube SPME-performed continuous extraction, concentration, desorption, and injection using an autosampler, is usually used in combination with high performance liquid chromatography and liquid chromatography-mass spectrometry. This technique has successfully been applied to the determination of various compounds such as pesticides, drugs, environmental pollutants, and food contaminants. In this review, an overview of the development of in-tube SPME technique and its applications to environmental, clinical, forensic, and food analyses are described.     

Monolithic columns in high-performance liquid chromatography

Monolithic media have been used for various niche applications in gas or liquid chromatography for a long time. Only recently did they acquire a major importance in high-performance column liquid chromatography (HPLC). The advent of monolithic silica standard- and narrow-bore columns and of several families of polymer-based monolithic columns has considerably changed the HPLC field, particularly in the area of narrow-bore columns. The origin of the concept, the differences between their characteristics and those of traditional packed columns, their advantages and drawbacks, the methods of preparation of monoliths of different forms, and the current status of the field are reviewed. The actual and potential performance of monolithic columns are compared with those of packed columns. Monolithic columns have considerable advantages, which makes them most useful in many applications of liquid chromatography. They are extremely permeable and offer a high efficiency that decreases slowly with increasing flow velocity.     

Design of the monolithic polymers used in capillary electrochromatography columns

Monolithic columns for capillary electrochromatography (CEC) are receiving quite remarkable attention. Both the simplicity of the in situ preparation and the large number of readily available chemistries make the monolithic separation media a vital alternative to capillary columns packed with particulate materials. This review summarizes the current state-of-the-art in this rapidly growing area of CEC with a focus on monolithic capillary columns prepared from synthetic polymers. Recent achievements in column technologies for both high-performance liquid chromatography and capillary electrophoresis are used as the starting point to highlight the influence of these well established analytical methods on the development of monolithic capillary columns for CEC. The effects of individual variables on the separation properties of monolithic capillaries are discussed in detail. The analytical potential of these columns is demonstrated with separations involving various families of compounds in different chromatographic modes.     

Gas-liquid chromatography of amino acids: Columns and methodology as a basis for routine amino acid analysis using glass capillary gas chromatography

A carefully Standardized technique is described for the preparation of glass capillary columns which can be used successfully for routine quantitative amino acid analysis. Comparison is made between two different modes of sample injection. Preliminary quantitative results from “split” injection and “on-column” injection techniques are evaluated statistically and it is concluded that the “on-column” system is a prerequisite for quantitative amino acid analysis by glass capillary gas chromatography. An analysis of fish muscle protein hydrolyzate illustrates an application of this technique and results are compared with those from a packed column analysis.     

毛细管电色谱整体柱制备新进展

毛细管电色谱整体柱以其制备相对简单,渗透性好,柱效高等优点,成为电色谱领域中的一个研究热点.主要包括有机聚合物型和硅基整体柱两种类型.其制备方法还不十分成熟,有待完善.     

High-throughput capillary gas chromatography for the determination of polychlorinated biphenyls and fatty acid methyl esters in food samples

High-throughput capillary gas chromatography (CGC) methods, developed during the Belgian 1999 "dioxin" food crisis, for the determination of the contaminating polychlorinated biphenyls (PCBs) and the fatty acid composition of the lipids are described. For PCB analysis, the fat obtained by ultrasonic extraction is fractionated by matrix solid-phase dispersion, and the PCBs are analyzed by CGC-electron capture detection on a 10-mL x 100-microm-i.d. HP-5MS column. Analytical conditions for the high-speed column are deduced from analyses on conventional CGC columns using the method translation software. The concept of retention time locking is implemented to facilitate the elucidation of the PCB markers. The fatty acid methyl esters (FAMEs) are prepared by the sodium methylate procedure on part of the ultrasonic extract followed by analysis on 10-mL x 100-microm-i.d. HP-WAX or BPX-70 capillary columns. By optimizing both the sample preparation and CGC analysis, the throughput is more than fifty PCB and FAME samples per day with the same robustness as conventional methods.     

Two-Dimensional Gas Chromatography. Concepts,Instrumentation, and Applications – Part 1: Fundamentals,Conventional Two-Dimensional Gas Chromatography,Selected Applications

The writer of this review published in 1978 a three-part article on two-dimensional gas chromatography in the first three issues of this journal [1]. The review was written at a time when capillary column GC was still in its infancy. Commercial columns were (essentially) unavailable and sample introduction into capillary columns was done exclusively in the split mode. Two-dimensional separations were explored in only a few laboratories. The limitations of capillary column technology made this exercise rather difficult. The introduction of fused silica capillary columns in the early eighties drastically changed the landscape in which gas chromatography was practiced. It took the chromatographic community just a few years to convert from packed columns to capillary columns. Instrumentation and accessories specifically designed for capillary column use came onto the market. This writer had great hopes that the revolution in capillary column GC would be mirrored in the development of instrumentation for Two-Dimensional Gas Chromatography. This never materialized. On the contrary, tentative steps taken by a few manufacturers and suppliers of chromatographic equipment fizzled out. It was perhaps the introduction of relatively inexpensive and user friendly GC/MS instrumentation, in combination with nearly indestructible fused silica capillary columns that took away the incentive to develop commercially viable Two-Dimensional Gas Chromatography. Much of the thinking went like this: why insist on good chromatography if mass spectrometry can do the job without the need for complete separation. Some progress in the further development of conventional Two-Dimensional Gas Chromatography has certainly been made over the last 20 years but there has not been a great deal of excitement. Applications have also been relatively sparse and they are limited to just a few areas. Science does not remain static and chromatography is no exception. Progress in gas chromatography is driven by new technology and ideas. Substantial improvements in two-dimensional GC were not forthcoming until Phillips and his research group introduced and implemented an entirely new form of Two-Dimensional Gas Chromatography, called comprehensive two-dimensional GC, or GC×GC. This breakthrough occurred only in 1991 [2]. It does take some time before scientists change attitudes and habits. There is always a time lag between the introduction of new technology and its general acceptance. The public's attitude toward comprehensive Two-Dimensional Gas Chromatography is probably no exception. The number of scientists who are actively pursuing this new branch of gas chromatography is still very small. It is often a single individual who carries the torch. J.B. Phillips' name is synonymous with comprehensive Two-Dimensional Gas Chromatography. He is not only its inventor and proponent but his fertile mind has initiated research in other related areas. Sadly, he passed away shortly before this review was written. This contribution is dedicated to his memory.     

新型有机-无机杂化整体柱的制备及其在毛细管液相色谱及加压毛细管电色谱中的应用

以丙烯酰胺(AM)为单体,八乙烯基倍半硅氧烷(POSS)为交联剂,偶氮二异丁腈(AIBN)为引发剂,四氢呋喃(THF)为致孔剂,通过原位聚合法制备了poly(POSS-co-AM)有机-无机杂化整体柱,并对各反应物的配比进行了优化。结果表明,当功能单体与致孔剂、POSS与AM的质量比均为1.0: 5.0, AIBN的质量分数为0.1%时,杂化整体柱的柱效最高。无机材料的引入使整体柱结构均匀并具有良好的渗透性,该整体柱既能用于亲水色谱模式,也能用于反相色谱模式。将制备的整体柱用于毛细管液相色谱和加压毛细管电色谱分离核苷类、胺类、硝基苯胺类等化合物,获得了良好的效果。