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Use of adsorbent and supercritical carbon dioxide to concentrate flavor compounds from orange oil

Shen, Z., Mishra, V., Imison, B., Palmer, M., Fairclough, R.
Journal of agricultural and food chemistry 2002 v.50 no.1 pp. 154-160
essential oils, oranges, flavor compounds, terpenoids, alcohols, aldehydes, extraction, carbon dioxide, pressure, adsorbents, silica gel, adsorption, supercritical fluid extraction
Orange oil is composed largely of terpene hydrocarbons but is a source of flavor and fragrance compounds (oxygenated) that are present in low concentrations. To increase the ratio of oxygenated compounds to terpene hydrocarbons, orange oil was partially fractionated by adsorption of the oxygenated compounds onto porous silica gel, with full utilization of its adsorbent capacity, and then further purified by desorption into supercritical carbon dioxide. The desorption of 24 compounds was monitored by GC and GC-MS. Adsorption alone removed three-fourths of the terpene hydrocarbons, and fractional extraction by supercritical carbon dioxide (SC-CO2) improved the separation further. Response surface methodology was used in the experimental design, and regression analysis was used to determine the effects of process variables. Extraction at low temperatures and flow rates improved separation by SC-CO2. Decanal was concentrated to 20 times that of the feed oil by using SC-CO2 at 13.1 MPa, 35 degrees C, and 2 kg/h. The systems were operating at close to equilibrium conditions because of the fine dispersal of the oils and the excellent mass transfer properties of supercritical carbon dioxide.