Optimization of Countercurrent Supercritical Fluid Extraction of Minor Components from Olive Oil

A process based on the use of a semi-continuous countercurrent supercritical fluid extraction (CC-SFE) has been optimized to concentrate minor components, with functional properties, from olive oil. The optimization of the main variables involved in the supercritical extraction process (extraction pressure, temperature and sample flow rate) was performed using a surface response methodology (RSM). A central composite circumscribed design (CCCD) was employed to study the responses selected to describe the process, such as the extraction yield, the concentration of the different minor compounds (squalene, sterols and tocopherols) in the CO2-rich upper current stream, and the recovery of these compounds from the olive oil. Parameters of the model, for each response variable, were simultaneously estimated by Partial Least Squares (PLS) regression. The statistical analysis of the results allowed obtaining mathematical models able to predict the behavior of the different responses selected as a function of the main variables involved in the process. The optimum conditions obtained, that maximized all the responses as a whole, were: extraction pressure, 234 bar; extraction temperature, 35°C and sample flow rate, 82 mL/h, working with a solvent flow rate equal to 2000 mL/h (S/F equal to 28.4 kg CO2/kg oil). The optimum of the model was experimentally confirmed allowing around 90% recovery of squalene without significant changes on the nutritional and physicochemical properties of the oil.