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Analysis of aqueous matrices using supercritical fluid extraction in conjunction with chromatographic spectroscopic and mass spectrometric techniquesMinty, Brian January 2004 (has links)
The use and supply of various organic solvents for analytical chemistry is coming under scrutiny due to their environmental impact. International legislation now prevents the supply of "ozone depleting" solvents for laboratory purposes. Consequently alternative analytical methods to those which had previously relied upon the use of a range of organic solvents need to be developed. Supercritical fluids exhibit some properties associated with gases and liquids, and in particular their solvating characteristics are equivalent to a wide range of conventional organic solvents. Environmentally benign carbon dioxide in its supercritical fluid state can be utilised to imitate the solvating power of a range of organic solvents from non polar pentane through to more polar pyridine. There are many reports detailing the use of supercritical fluid extraction for the isolation of target compounds from a very wide range of solid matrices. The objective of these studies was to develop direct liquid supercritical fluid extraction procedures using carbon dioxide to isolate, concentrate and quantify target analytes from aqueous media. These investigations involved using off-line and on-line supercritical fluid extraction procedures with final analytical detection and quantification being accomplished using a range of chromatographic, spectroscopic and mass spectrometric methods. Within chapters 2 and 3, an alternative infrared method for determining the quantity of oil in process and discharge waters is described. The results of quantification studies involving various oils and hydrocarbons indicate that the custom built supercritical fluid extraction system developed for these investigations directly coupled with an infrared spectrometer provide an alternative method to traditional liquid-liquid extraction procedures that involve the use of ozone depleting and/or toxic organic solvents. Chapter 4 describes how direct aqueous supercritical fluid extraction was used to continuously isolate free testosterone as it was liberated during the enzymic digest of a testosterone-/3-D-glucuronide solution incubated with Helix pomatia glucuronidase. Other studies described within this chapter that also involved the use of direct aqueous supercritical fluid extraction with off-line gas chromatography-mass spectrometry describe procedures for determining trace levels of organophosphate pesticides and polyaromatic hydrocarbons in aqueous samples. The development and use of on-line direct aqueous supercritical fluid extraction coupled with supercritical fluid chromatography-mass spectrometry using atmospheric pressure chemical ionisation for the analysis of phenols at the ppb level is described in Chapter 5. Chapter 6 describes the use of direct aqueous supercritical fluid extraction coupled online with liquid chromatography-mass spectrometry using ammonia chemical ionization for the analysis of three veterinary drugs at the ppb level. Results of off-line and on-line studies involving electrospray tandem mass spectrometry with high pressure liquid chromatography for the analysis of a range of ionophores at the low ppb level following their isolation using direct aqueous supercritical fluid extraction are also presented.
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Applications of modifiers in supercritical fluid extraction and chromatograph /Mulcahey, Leah J., January 1991 (has links)
Thesis (Ph. D.)--Virginia Polytechnic Institute and State University, 1991. / Vita. Abstract. Includes bibliographical references (leaves 167-170). Also available via the Internet.
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Supercritical fluid extraction of mogrosides from Siraitia grosvenoriiXia, Yan, 1971- January 2006 (has links)
No description available.
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Supercritical fluid extraction of mogrosides from Siraitia grosvenoriiXia, Yan, 1971- January 2006 (has links)
Mogrosides, the main active components in S. grosvenorii SWINGLE, are considered to be some 250 times sweeter than sucrose and to possess several medicinal attributes. Previous isolation processes used large quantities of toxic solvent that resulted in toxic residues of organic solvent in this high value food. Supercritical fluids fulfill the requirements of non-toxicity, recycle ability, and useful solvent characteristics. The work presented in this thesis is directed to the extraction of mogrosides from the powdered S. grosvenorii concentrate (SG) and the crude extract after resin treatment (MG) with sub critical water and supercritical CO2. / Because no source of mogroside V reference material is available commercially, the first objective of this research was to isolate mogroside V of sufficient purity that it could be crystallized. This objective was achieved by selecting suitable eluates from resin chromatography coupled with preparative thin layer chromatography (TLC). Crystalline white isolate was further characterized by 13C-NMR and by MS and determined to be mogroside V, which was suitable as a reference material for subsequent experiments. / The process variables for both sub critical water and supercritical carbon dioxide extraction were evaluated and optimized so that conclusions could be formulated regarding the relative merits of the two proposed extraction methods. The efficiency of extraction was determined spectrophotometrically based on the recovery of mogrosides from the starting material following the vanillin-HClO4 method. / When compared with Soxhlet solvent extraction, supercritical fluid extraction with either sub critical water or supercritical CO2 provided improved recoveries and consumed less organic solvent. In addition, the purity of the extracts differed greatly. For identical SG samples, sub critical water extraction was demonstrated to be more efficient (62.4% recovery) compared with 37.0% recovery by EtOH modified scCO2 extraction or 5.1% for Soxhlet extraction with hexane.
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Comparative studies on the physical and surface properties of salmeterol xinafoate prepared by spray drying and supercritical fluid processing. / CUHK electronic theses & dissertations collectionJanuary 2003 (has links)
Tong Hoi Yee. / "July, 2003." / Thesis (Ph.D.)--Chinese University of Hong Kong, 2003. / Includes bibliographical references (p. 237-253). / Electronic reproduction. Hong Kong : Chinese University of Hong Kong, [2012] System requirements: Adobe Acrobat Reader. Available via World Wide Web. / Mode of access: World Wide Web. / Abstracts in English and Chinese.
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Leaching of active ingredients from blueberries and cranberries using supercritical carbon dioxide and ethanol as an entrainer and analyzing using GC/MSElsayed, Nada H. January 2009 (has links)
Thesis (M.S.B.E.)--University of South Florida, 2009. / Title from PDF of title page. Document formatted into pages; contains 108 pages. Includes bibliographical references.
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