Author
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King, Jerry |
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Taylor, Scott |
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BLANCO, MIGUEL - UNIV OF CADIZ, SPAIN |
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Submitted to: Meeting Abstract
Publication Type: Abstract Only Publication Acceptance Date: 6/4/1999 Publication Date: N/A Citation: N/A Interpretive Summary: Technical Abstract: Scaling up supercritical fluid chromatography (SFC) for preparative and process applications requires optimization of sample preparation, selection of pressure and temperature, and choice of cosolvent and column sorbent. In this study, these factors were examined to purify mixtures containing phospholipids. Studies on analytical scale SFC indicated that a silica column with 25 vol.% ethanol:water/9:1 modifier at 350 bar and 50 deg C migrated and separated three of four phospholipid standards. Sorbent type was optimized using an Isco SFX-3560 extractor for preparative SFC to collect lecithin fractions using a range of conditions: pressure (350-500 bar), temperature (50-80 deg C), different modifiers (up to 40 vol.%), and sorbents (silica gel, aluminas, diatomaceous earths, bentonites, amino-bonded silicas). Elution order of solutes varied with sorbent; neutral alumina was preferable for early elution of phosphatidylcholine. Scale up to a larger SFC column was accomplished using silica gel and alumina columns by lowering modifier concentration (ethanol:water/9:1) and increasing total eluent volume for fractionation. These scaled up SFC conditions were used with a supercritical fluid extraction (SFE) pretreatment (645 atm, 80 deg C, 15 mole % ethanol, 400 L CO2 NTP) to process deoiled soy flakes for phospholipids. This SFE/SFC process utilized a neutral alumina column at 340 atm, 50 deg C, a 9:1/ethanol:water modifier in a step wise gradient, to isolate phospholipids. Using environmentally benign supercritical fluid CO2 for extraction and chromatography and minimizing solvents are advantages of this process. |
