Process for the recovery of a phytolipid composition

A process for preparing a phytolipid composition comprising squalene, phytosterols, tocopherols and vegetable wax which comprises the steps of:

• (1) distilling a vegetable oil by-product comprised of mixed tocols, fatty acids, hydrocarbons, vegetable waxes, sterol esters of fatty acids, sterols, triterpenoid alcohols, squalene, methyl-sterols, and mono-, di-, and triglycerides at a temperature of about 170 to about 320° C. and a pressure of about 0.1 to about 35 torr to produce (i) a vapor product comprising fatty acids and low boiling hydrocarbons and (ii) a liquid product;
• (2) distilling the liquid product of step (1) at a temperature of about 230 to about 300° C. and a pressure of about 0.0005 to about 1 torr to produce (i) a second vapor product comprising a mixed tocols concentrate, squalene, phytosterols, and vegetable wax and (ii) a second liquid product;
• (3) condensing the vapor product and mixing the condensed vapor product with an extractant of an alkanol or a mixture of acetone and water to form a mixture, separating the mixture into two phases comprising (i) a first phase comprising a majority of the extractant and (ii) a second phase comprising a majority of the condensed vapor product;
• (4) collecting the second phase formed in step (3) and removing the extractant employed in step (3);
• (5) cooling the first phase formed in step (3) to effect formation of a precipitate followed by collection of the precipitate and removal the of the extractant employed in step (3);
• and
• (6) combining the second phase collected in step (4) with the precipitate collected in step (5),
• whereby a phytochemical composition comprising about 10 to about 40 weight percent squalene, about 2 to about 20 weight percent phytosterols, about 1 to about 10 weight percent of mixed tocols and about 40 to about 80 weight percent vegetable wax is obtained.

A process for preparing a phytochemical composition comprising squalene, phytosterols, tocopherols and vegetable wax which comprises the steps of:

• (1) distilling a rice bran oil by-product comprised of mixed tocols, fatty acids, hydrocarbons, vegetable waxes, sterol esters of fatty acids, sterols, triterpenoid alcohols, squalene, methyl-sterols, and mono-, di-, and triglycerides at a temperature of about 240 to about 290° C. and a pressure of about 0.2 to about 20 torr to produce (i) a vapor product comprising fatty acids and low boiling hydrocarbons and (ii) a liquid product;
• (2) distilling the liquid product of step (1) at a temperature of about 230 to about 260° C. and a pressure of about 0.005 to about 0.5 torr to produce (i) a second vapor product comprising a mixed tocols concentrate, squalene, phytosterols, and vegetable wax and (ii) a second liquid product;
• (3) condensing the vapor product and mixing the condensed vapor product with an extractant selected from the group consisting of methanol, ethanol, propanol, and 2-propanol wherein the volume:volume ratio of extractant:condensed vapor product is about 6:1 to 12:1 separating the mixture into two phases comprising (i) a first phase comprising a majority of the extractant and (ii) a second phase comprising a majority of the condensed vapor product;
• (4) collecting the second phase formed in step (3);
• (5) cooling the first phase formed in step (3) to effect formation of a precipitate followed by collection of the precipitate;
• and
• (6) combining the second phase collected in step (4) with the precipitate collected in step (5) and heating the materials collected in steps (4) and (5) at a temperature of about 50 to about 100° C. and a pressure of about 200 to about 1 Torr to remove extractant employed in step (3),
• whereby a phytolipid composition comprising about 15 to about 35 weight percent squalene, about 3 to about 15 weight percent phytosterols, about 2 to about 8 weight percent of mixed tocols, about 45 to about 75 weight percent vegetable wax and less than about 0.1 weight percent extractant/solvent is obtained.