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Continuous extraction of squalene from shark liver oil using supercritical carbon dioxide was carried out in both laboratory and pilot scale plant. The shark liver oil contained around 50% by weight squalene, which was recovered as the main extract stream. The other major components in the oil were triglycerides, which were recovered as raffinate, and pristane, which was recovered as a second extract stream. Separation performance was determined as a function of temperature; pressure; oil to carbon dioxide flow rate ratio, packed height and type of packing; and reflux ratio. The pressure, temperature, and feed oil concentration of squalene determined the maximum loading of oil in carbon dioxide. The oil to carbon dioxide ratio determined the squalene concentration in both the product stream and raffinate stream. The ratio of oil flow rate to the flow rate of squalene required to just saturate carbon dioxide was found to be a useful correlating parameter for the oil loadings and product compositions. Of the three packings investigated, wire wool gave the best separation efficiency and Raschig rings the worst efficiency. Mass transfer correlations from the literature were used to estimate the number of transfer units NTU from experimental data and literature correlations. NTU's from the experimental data were comparable to predictions at a pilot scale but were underpredicted at the laboratory scale. The use of reflux at the pilot scale enabled the concentration of squalene in the product stream to be increased from 92% by mass to a maximum of 99% by mass at fractionation conditions of 250 bar and 333 K.

Ginger, black pepper, and chili powder were extracted using near-critical carbon dioxide, propane, and dimethyl ether on a laboratory scale to determine the overall yield and extraction efficiency for selected pungent components. The temperature dependency of extraction yield and efficiency was also determined for black pepper and chili using propane and dimethyl ether. The pungency of the extracts was determined by using an NMR technique developed for this work. The volatiles contents of ginger and black pepper extracts were also determined. Extraction of all spice types was carried out with acetone to compare overall yields. Subcritical dimethyl ether was as effective at extracting the pungent principles from the spices as supercritical carbon dioxide, although a substantial amount of water was also extracted. Subcritical propane was the least effective solvent. All solvents quantitatively extracted the gingerols from ginger. The yields of capsaicins obtained by supercritical CO(2) and dimethyl ether were similar and approximately double that extracted by propane. The yield of piperines obtained by propane extraction of black pepper was low at approximately 10% of that achieved with dimethyl ether and CO(2), but improved with increasing extraction temperature.

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Solubility measurements for squalene, vitamin A palmitate, orange roughy oil, spiny dogfish liver oil, and commercial cod liver oil in supercritical carbon dioxide are reported over the temperature range 313−333 K and pressure range 200−300 bar. Solubility measurements are also reported for squalene, orange roughy oil, spiny dogfish liver oil, and cod liver oil in supercritical carbon dioxide + ethanol mixtures over the pressure range 200−300 bar at 333 K, and ethanol mass concentrations up to 12% by mass on a solute free basis. The use of ethanol as an entrainer substantially increased the solubility of all fish oil components. The increase in solubility, S, with ethanol concentration at fixed temperature and pressure was correlated by the empirical equation S = S 0 exp(kX), where S 0 is the solubility in pure CO2 at given temperature and pressure, k is a fitted constant, and X is the mass fraction of ethanol on a solute-free basis.

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