Analysis With Supercritical Fluids Extraction And Chromatography

The use of supercritical fluids in analytical chemistry is still grow ing. More and more analysts are discovering the favorable advan tages for a number of applications. Especially supercritical fluid extraction (SFE) has attracted a lot of interest in recent years due to its simplicity. Supercritical fluid chromatography (SFC) has become better established and the development of this technique has been accelerated by the many applications with capillary col umns which have been published in the literature. At first SFC equipment was based on instruments commonly used for liquid chromatography, and the first commercial in struments were derived from this technology. However, capillary columns can be much more easily interfaced to gas chromatogra phy equipment especially to the detectors commonly used for Oc. Many stationary phases both for packed micro columns and capillary columns have been designed for SFC purposes extending this technology to LC and OC. The most common fluid applied in SFC and SFE is carbon dioxide. The advantages of supercritical CO , such as having dif 2 fusivity like a gas and solvating power depending on temperature and pressure, are also valid for other fluids and modified fluids. Both properties are valuable for sample extraction and extraction selectivity.

The editor has brought together in a compact and readable form the new methods of analytical chemistry using supercritical fluids. The volume provides comprehensive treatment of supercritical fluid chromatography (SFC) and supercritical fluid extraction (SFE); it discusses both theory and practice. The contributions are written by leading experts in their fields with exhaustive practical experience in SFC and SFE. Special attention is given to the description of applications and thus provides the experienced analyst with invaluable information widely scattered in the literature and helps the novice to adopt these new techniques quickly in his laboratory. An addendum includes brand new literature on SFC and SFE.

The continued search for rapid, efficient and cost-effective means of analytical measurement has introduced supercritical fluids into the field of analytical chemistry. Two areas are common: supercritical fluid chroma tography and supercritical fluid extraction. Both seek to exploit the unique properties of a gas at temperatures and pressures above the critical point. The most common supercritical fluid is carbon dioxide, employed because of its low critical temperature (31 °C), inertness, purity, non-toxicity and cheapness. Alternative supercritical fluids are also used and often in conjunction with modifiers. The combined gas-like mass transfer and liquid-like solvating characteristics have been used for improved chroma tographic separation and faster sample preparation. Supercritical fluid chromatography (SFC) is complementary to gas chro matography ( GC) and high performance liquid chromatography (HPLC), providing higher efficiency than HPLC, together with the ability to analyse thermally labile and high molecular weight analytes. Both packed and open tubular columns can be employed, providing the capability to analyse a wide range of sample types. In addition, flame ionization detection can be used, thus providing 'universal' detection.

by Professor D. E. Games, Mass Spectrometry Research Unit, University College of Swansea Sample preparation can be viewed as occupying a Cinderella role in analytical science. However, the quality of sample preparation plays a key role in high In the past decade, there has been quality analysis and deserves higher stature. considerable interest in the use of supercritical fluid extraction (SFE) as an alternative to conventional procedures for the preparation of samples for ana lysis. The driving force for this development is the need for automated, sim pler, faster, non-destructive and selective methods for extraction, preferably using non-toxic extraction media which are easily disposed of. Utilization of supercritical fluids for extraction fulfils these requirements because of their unique physical chemical properties and usually low toxicity. Selectivity can be achieved by suitable selection of pressure (density), temperature and modi fier conditions which enable solvating power to be varied. The high diffusivity of supercritical fluids provides rapid sample penetration and extraction. Use of fluids with low critical temperatures enables extraction to be conducted under mild thermal conditions ensuring that thermally labile compounds do not decompose. The technique can be used off-line, and the extracts analysed by appropriate techniques, or it can be used on-line, by coupling with a variety of chromatographic techniques. These can then, if necessary, be coupled fur ther with spectroscopic techniques, such as Fourier transform infrared, ultra violet or mass spectrometry, to provide specific identification or structural information.

An exploration of fundamental as well as practical aspects of supercritical fluid chromatography and extraction. It addresses topics such as: packed columns in SFC; detection in SFC; supercritical fluid chromatography/mass spectroscopy; and evaporative light scattering detection in SFC.

During the past decade supercritical fluid extration (SFE) has attracted considerable attention as a sample preparation procedure in analytical chemistry. The successful implementation of this technique can lead to improved sample throughput, more efficient recovery of analytes, cleaner extracts, economic replacement of halogenated solvents and a high level of automation, compared to conventional sample preparation procedures. This book provides an overview of basic principles of SFE as well as in-depth reviews of both on- and off-line SFE methods. The on-line coupling of SFE with both chromatographic and spectroscopics techniques has been the subject of a great deal of research effort and is dealt with in detail. Newer developments, such as off-line SFE of solid and liquid matrices, are starting to attract a great deal of interest, and the coverage of these areas will prove of particular value to the analytical chemist. The international team of authors has illustrated these topics with many `state-of-the-art' applications, and each chapter provides a comprehensive list of references. For the convenience of the reader, an appendix which contains pressure conversion scales and supercritical fluid carbon dioxide density tables appears at the end of the book. The volume's extensive coverage of both on-line and off-line extraction will be particularly useful to analytical chemists, in a wide range of environments, seeking to develop high quality, simple and robust SFE methods.

Thermodynamics of supercritical fluids with respect to lipid-containing systems; Solubility measurement of lipid constituents in supercritical fluids; Supercritical fluid extraction of oilseeds/lipids in natural products; Supercritical fractionation of lipids; Oilseed solubility and extraction modeling; Modeling of the supercritical fluid extraction rate of oilseeds; Design and economic analysis of supercritical fluid extraction processes; Supercritical fluid extraction and fractionation of fish oils; Supercritical fluid extraction of egg lipids; Supercritical fluid extraction of Cocoa and Cocoa products; Superctitical CO2 extraction of meat products and edible animal fats for cholesterol reduction; Supercritical fluid extraction of algae; Effect of supercritical fluids on residual meals and protein functionality; Treatment of food materials with supercritical carbon dioxide; Enzymatic synthesis in supercritical fluids; Basic principles and the role of supercritical fluid chromatography in lipid analysis; Supercritical fluid chromatography for the analysis of oleochemicals; Supercritical fluid chromatography of trace components in oils and fats; Analytical supercritical fluid extraction for oil and lipid analysis.

By encouraging a deliberate, systematic approach to supercritical fluid extraction (SFE) methods and techniques, this book enables scientists and technicians to avoid disappointing results and erroneous conclusions and develop reliable guidelines for using this versatile technology.