Recovery of phytosterols from sunflower oil deodorizer distillates

Phytosterols are usually recovered by crystallization from the deodorizer distillate (DD) of vegetable oils. In this work, the impact of the principal process variables (viz., solvents and cosolvents, cooling rate, crystallization temperature, and ripening time) on the quality and yield of the recovered phytosterols was studied by using a sunflower oil DD "enriched" (i.e., preconcentrated) via transesterification with ethanol (EDD as a feedstock and commercial hexane as solvent (S), with S/EDD mass ratios of 3 to 5. Water (0 to 4.5 wt%) and ethanol (0 to 10 wt%) were used as cosolvents, with crystallization temperatures between 0 and -20degreesC and crystallization times from 4 to 96 h. The cooling rate was either -20degreesC/h or "brisk chilling" from 40 to -5degreesC. The nature and composition of the EDD solvent and cosolvent composite arose as the most important process variable, strongly influencing both the percentage of sterol yield and the purity of the crystals, as well as their filterability and washability. Water-saturated hexane sufficed to give good crystallization, yet the beneficial effect of adding water as the single cosolvent was enhanced by adding small and precise amounts of ethanol. A recovery of sterols as high as 84% (with 36% purity) was achieved by using a single-stage batch crystallization of the S/EDD mixture (S/EDD = mass ratio 4).