Supercritical fluid chromatography development

A method which uses supercritical fluid/solid phase extraction/supercritical fluid chromatography (SE/SPE/SEC) has been developed for the analysis of trace constituents in complex matrices (67). By using this technique, extraction and clean-up are accomplished in one step using unmodified SC CO2. This step is monitored by a photodiode-array detector which allows fractionation. Eigure 10.14 shows a schematic representation of the SE/SPE/SEC set-up. This system allowed selective retention of the sample matrices while eluting and depositing the analytes of interest in the cryogenic trap. Application to the analysis of pesticides from lipid sample matrices have been reported. In this case, the lipids were completely separated from the pesticides. 

Supercritical fluid chromatography (SFC) provides a means of minimizing the limitations of CSPs developed for FC while retaining the impressive chiral selectivity that has been achieved through the evolution of CSPs during the past two decades [6, 7]. The use of supercritical fluids as eluents for chromatographic separations was... 

Principles and Characteristics Klesper et al. [14] have introduced supercritical fluid chromatography (SFC). The oil industry has been a major force in the development of many aspects of the application of supercritical fluids. Much of the pioneering development of SFC was carried out by Sie and Rijnders [231,232], who also coined the term supercritical fluid chromatography [233]. 

In supercritical fluid chromatography, fluids above their critical point are used as mobile phases. This chapter discusses the principles of operation, mobile phase considerations, parameters that can be adjusted in method development as well as an overview of instrumentation required and a few pertinent examples from current literature. Not everything can be illustrated, but the advantages of this diverse technology will be highlighted. 

Zhao, Y., Woo, G, Thomas, S., Semin, D., Sandra, P. Rapid method development for chiral separation in drug discovery using sample pooling and supercritical fluid chromatography-mass spectrometry. J. Chromatogr. A 2003, 1003, 157-166. 

ViUeneuve, M.S., Anderegg, R.J. Analytical supercritical fluid chromatography using fully automated column and modifier selection valves for the rapid development of chiral separations. J. Chromatogr. A 1998, 826, 217-225. 

To apply a screening approach to proactive method development, analyses of selectivity samples under a variety of mobile phase conditions are conducted on different HPLC columns. HPLC columns should be as orthogonaT as possible and variations in solvent composition should be designed to maximize the probability of selectivity differences. Alternate separation techniques, such as ion exchange chromatography (IC), supercritical fluid chromatography (SFC), or capillary electrophoresis (CE) may also be used to obtain orthogonality. 

Supercritical fluid chromatography (SFC) is an intermediate chromatographic technique between GC and HPLC. It depends upon the fact that when a fluid becomes supercritical (both the temperature and pressure are at or above its critical point) it develops some of the solvating properties of a liquid whilst retaining the low viscosity of a gas. Hence, mass transfer (essential to efficient chromatography) is more akin to that of GC than HPLC, but many compounds can be chromatographed at temperatures much lower than what would be required by GC, so some thermally labile compounds are amenable to SFC where they would degrade under GC conditions [28]. 

The prerequisites for the use of gas chromatography as an analytical tool in enantiomer analysis, i.e., quantitative resolvability, substrate volatility and thermal stability, tend to restrict its general use. The development of supercritical fluid chromatography (SFC) for enantiomer... 

Supercritical fluid chromatography (SFC) is a relatively recently developed chromatographic technique. Because of its ability to deal with compounds that are either polar or of high molecular weight, much attention has recently focused on applications of SFC to the analysis of different analytes using a variety of fluids or fluid mixtures to provide differing solvent capabilities and select vities. As a result there is a large amount of research currently underway both in SFC method development and in hardware development. 

The specific development of a batch process is illustrated in the following example, namely the separation of the enantiomers of racemic trans-stilbene oxide (TSO) [28], For this example, supercritical fluid chromatography was particularly appropriate for the resolution. 

Chemists in its Methods of Analysis, 8th ed. Methods have also been developed for DON by TLC (93) and for several trichothecenes both by immunoassay (94,95) and by supercritical fluid chromatography (96). In comparison with LC, supercritical fluid chromatography is characterized by sharper peaks and faster analysis times, similar to those obtained by capillary GC. 

Many reports (78-84) investigated the differences in packed and capillary supercritical fluid chromatography. Unfortunately, the rift between packed and capillary column users of SFC impeded the development of the science. This rift is a likely cause of the current low interest in SFC. Ideally, the unique features of the mobile phase is the area of scientific exploration that should be exploited. Choice of column size or type should be dependent upon the analytical problem to be solved. 

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