Extractants supercritical fluid

Supercritical Fluid Extraction. Supercritical fluid (SCF) extraction is a process in which elevated pressure and temperature conditions are used to make a substance exceed a critical point. Once above this critical point, the gas (CO2 is commonly used) exhibits unique solvating properties. The advantages of SCF extraction in foods are that there is no solvent residue in the extracted products, the process can be performed at low temperature, oxygen is excluded, and there is minimal protein degradation (49). One area in which SCF extraction of Hpids from meats maybe appHed is in the production of low fat dried meat ingredients for further processed items. Its apphcation in fresh meat is less successful because the fresh meat contains relatively high levels of moisture (50). 

Separation Techniques. Current methods for separating fatty acids are by solvent crystaUi2ation or by the hydrophili2ation process. Other methods that have been used in the past, or perhaps could be used in the future, are panning and pressing, solvent extraction, supercritical fluid extraction, the use of metal salts in assisting in separation, separations using urea complexes, and adsorption/desorption. 

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. 

K. Haitonen and M. L. Riekkola, Detection of /3-blockers in urine by solid-phase extraction-supercritical fluid exti action and gas cliromatogi aphy-mass spectrometi y , 7. Chromatogr. B 676 45-52 (1996). 

D. A. Roston, Supercritical fluid extraction-supercritical fluid cliromatography for analysis of a prostaglandin HPMC dispersion . Drug Dev. Ind. Pharm. 18 245-255 (1992). 

Q. L. Xie, K. E. Markides and M. L. Lee, Supercritical fluid extraction-supercritical fluid clrromatogi aphy with fraction collection for sensitive analytes , 7. Chromatogr. Sci. 27 365-370(1989). 

Figure 15.14 Separation of explosives exnacted from water by using SPE-SFE-GC at several SEE trapping temperatures, peak identification is as follows NG, nitroglycerin 2,6-DNT, 2,6-dinitrotoluene 2,4-DNT, 2,4-dinitrotoluene TNT, triniti otoluene IS, 1,3-tiichloroben-zene. Adapted Journal of High Resolution Chromatography, 16, G. C. Slack et al., Coupled solid phase extraction supercritical fluid extraction-on-line gas cliromatography of explosives from water , pp. 473-478, 1993, with permission from Wiley-VCH.

Extraction of neonicotinoid residues from soil is much more difficult than their extraction from plant or water samples. Soil residues could exist as bound residue . Various extraction methods such as organic solvent extraction, supercritical fluid extraction (SEE), Soxhlet extraction and sonication have been used. Some extraction methods are described in the following. 

In liquid-solid extraction (LSE) the analyte is extracted from the solid by a liquid, which is separated by filtration. Numerous extraction processes, representing various types and levels of energy, have been described steam distillation, simultaneous steam distillation-solvent extraction (SDE), passive hot solvent extraction, forced-flow leaching, (automated) Soxh-let extraction, shake-flask method, mechanically agitated reflux extraction, ultrasound-assisted extraction, y -ray-assisted extraction, microwave-assisted extraction (MAE), microwave-enhanced extraction (Soxwave ), microwave-assisted process (MAP ), gas-phase MAE, enhanced fluidity extraction, hot (subcritical) water extraction, supercritical fluid extraction (SFE), supercritical assisted liquid extraction, pressurised hot water extraction, enhanced solvent extraction (ESE ), solu-tion/precipitation, etc. The most successful systems are described in Sections 3.3.3-3.4.6. Other, less frequently... 

S.B. Hawthorne, C.B. Grabanski, E. Martin and D.J. Miller, Comparison of Soxhlet extraction, pressurized liquid extraction, supercritical fluid extraction and subcritical water extraction for environmental solids recovery, selectivity and effects on sample matrix. J. Chromatogr.A 892 (2000) 421 133. 

Applications for SCF Extraction Supercritical fluid extraction has been mainly used for the extraction of natural extracts for aromatic substances and essences, and for various active substances for pharmaceuticals. Alternative possibilities include... 

Analytes can be separated from complex matrices by sample preparation techniques that include liquid extraction, supercritical fluid extraction, and solid-phase extraction. Dilute ionic analytes can be preconcentrated by adsorption onto an ion-exchange resin. Nonionic analytes can be concentrated by solid-phase extraction. Derivatization transforms the analyte into a more easily detected or separated form. 

U. Ullsten and K. E. Markides, Automated on-line solid phase adsorption/supercritical fluid extraction/supercritical fluid chromatography of analytes from polar solvents , J. Micmcolumn Sep. 6 385-393 (1994). 

E. Ibanez, J. Palacios and G. Reglero, Analysis of tocopherols by on-line coupling supercritical fluid extraction-supercritical fluid chromatography , J. Microcolumn Sep. 11 605-611 (1999). 

Solvent extraction Microwave extraction Solid phase microextraction Subcritical water extraction Subcritical water extraction Supercritical fluid extraction... 

Supercritical fluid extraction Supercritical fluid extraction... 

Soils, sediments, and solid wastes are mixed with anhydrous Na2S04 and extracted with methylene chloride by sonication or Soxhlett extraction. Supercritical fluid extraction (SEE) may be performed using C02 under the following conditions (Supelco, 1995) ... 

Extraction of solid samples Homogenization extractions Sonication extractions Microwave assisted extractions Soxhlet extractions Accelerated solvent extractions Supercritical fluid extractions Extraction of liquid samples Liquid-liquid extractions Solid phase extractions (SPE)... 

Zorita, S., R.Westbom, L.Thorneby, E. Bjorklund, and L. Mathiasson. 2006. Development of a combined solid-phase extraction-supercritical fluid extraction procedure for the determination of polychlorinated biphenyls in wastewater. Anal. Sci. 22 1455-1459. 

This chapter covers techniques for the extraction of semivolatile organics from solid matrices. The focus is on commonly used and commercially available techniques, which include Soxhlet extraction, automated Soxhlet extraction, ultrasonic extraction, supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), and microwave-assisted extraction (MAE). The underlying principles, instrumentation, operational procedures, and selected applications of these techniques are described. In a given application, probably all the methods mentioned above will work, so it often boils down to identifying the most suitable one. Consequently, an effort is made to compare these methodologies. 

While it is wonderful to be able to inject neat samples directly, sample preparation can often improve selectivity and sensitivity. If the resolution is poor, the salt content of the sample too high, or the capillary fouls, consider a sample cleanup. This can include liquid-liquid extraction, solid-phase extraction, supercritical fluid extraction, protein precipitation, or dialysis, depending on the solutes and application [38]. The final sample diluent should be a solution that is CE-Mendly. That usually means low ionic strength compared to the BGE. 

Ramsey, E.D., Perkins, J.R., Games, D.E., and Startin, J.R. 1989. Analysis of drug residues in tissue by combined supercritical-fluid extraction-supercritical-fluid chromatography-mass spectrometry-mass spectrometry. Journal of Chromatography, 464 353-64. 

Keywords Pressurized liquid extraction supercritical fluid extraction ultra-sound-assisted extraction microwave-assisted extraction matrix solid-phase extraction high-performance liquid chromatography gas chromatography liquid-liquid extraction solid phase extraction column chromatography... 

The preparation of high-purity tocopherols and phytosterols involves steps such as molecular distillation, adduct formation, liquid-liquid extraction, supercritical fluid extraction, saponification, and chromatography (175). The extraction of tocopherols from soybean oil deodorizer distillate by urea inclusion and saponification of free fatty acids resulted in good recovery of tocopherols (208). To improve the separation of sterols and tocopherols, Shimada et al. (209) used a lipase to esterify sterols with free fatty acids. Then the steryl esters and tocopherols were separated better by molecular distillation. Chang et al. (210) used supercritical fluid CO2 extraction to recover tocopherols and sterols from soybean oil deodorizer distillate. A patent by Sumner et al. (211) advocated treatment of the distillate with methanol to converted free fatty acids and other fatty acid esters to methyl esters that can then be removed by a stripping operation. Then separation of sterols and tocopherols could be carried out by molecular distillation. 

Supercritical fluid extraction Supercritical fluid extraction (SFE) uses compressed gas as the extraction medium and circumvents some of the problems associated with the use of classical separation techniques involving organic solvents. This technique combines features of distillation (i.e., separation because of differences in component volatiles) and liquid extraction (i.e., separation of components that exhibit little difference in their relative volatilities or that are thermally labile). A number of gases, when compressed isothermally at a temperature greater than their critical temperature and to pressures greater than their critical pressure, exhibit an enhanced solvating power (136), which has been known since the nineteenth century (137, 138), but its actual applications did not come to practice until the late twentieth century. 

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