Patent ID: 8247615
Filing Date: 2012-08-21
Classification: A23L,A61K,A61Q,C07C,C09B

Abstract:
1. A method for converting esterified xanthophylls from Capsicum into their non-esterified form comprising the steps of: a) contacting xanthophyll esters in an oleoresin with a hydrocarbon, with an oleoresin to hydrocarbon ratio of 1:0.5 to 1:10 (weight/weight), wherein the hydrocarbon is hexane or a mixture of low boiling hydrocarbons; b) adding an alcohol at an oleoresin:alcohol ratio of 1:1 to 1:10 (weight/weight); c) adding a base at an oleoresin:base ratio of 10:1 to 1:1 (weight/weight); d) applying a blanket of an inert gas, selected from, but not limited to nitrogen and argon; e) applying heat, if necessary, to at least 20° C. up to reflux temperature; f) allowing the mixture to stir and/or reflux under the inert atmosphere for 0.25 to 120 hrs; g) reducing the temperature of the reaction mixture to 0° to 50° C.; h) allowing the mixture to settle for 0.1 to 1000 hours; i) removing the upper hydrocarbon phase rich in carotenes, including alpha-carotene, beta-carotene, lycopene, and the xanthophyll, beta-cryptoxanthin; j) optionally adding more hydrocarbon to the remaining reaction mixture with stirring and repeating steps h) and i); k) desolventizing the upper hydrocarbon phase(s) to obtain a carotene concentrate; l) adding water, optionally mixed with an alcohol and/or complexing or chelating agent, to the lower phase remaining after hydrocarbon removal, with an oleoresin:water ratio of 1:0.1 to 1:5 (weight/weight), then thoroughly mixing; m) allowing the system to settle undisturbed for 0.5 to 1000 hours; n) draining the lower aqueous phase (first water wash) rich in soaps and other polar soluble materials; o) optionally repeating steps l) through n), one or more times; p) adding an alcohol to the mixture, optionally adjusting the water content of the mixture to 1-15%, by alcohol addition and/or concurrent or subsequent distillation; q) optionally removing the remaining hydrocarbon via distillation; r) separating the solid precipitated xanthophylls from the liquid supernatant by decanting, centrifugation, or filtration; s) adding to the solid xanthophylls, a wash solvent and mixing to form a slurry; t) separating the solid xanthophylls from the wash solvent, by decanting or centrifuging; u) optionally repeating steps s) and t) until the required purity is achieved; v) removing the solvent(s) and drying; w) packaging the dried xanthophylls obtained in the preceding step in an inert environment, selected from vacuum packaging or packaging inerted with nitrogen or argon; x) optionally, precipitating more solid xanthophylls from the liquid supernatant generated in steps r) and t) by addition of water and/or allowing the supernatant to stand for one or more days, and isolating the precipitate thereby formed by filtration, centrifugation, and/or decantation; y) optionally repeating step x) until no more precipitate is formed; and z) optionally desolventizing at step x) to recover the xanthophylls; aa) optionally adding an antioxidant to the mixture prior to desolventizing at steps v), and/or x) and/or z); ab) optionally extracting the xanthophylls from the precipitate at steps v), and/or x), and/or z) with a suitable solvent such as methylene chloride prior to desolventization; and ac) optionally adding water to the precipitate in step ab) prior to extracting; ad) optionally raising the temperature of the mixture to 40° to 60° after draining the water in step n) and isolating the zeaxanthin rich precipitate layer which forms at the bottom of the vessel; ae) optionally repeating steps z), aa), ab) and/or ac) with the precipitate layer formed in step ad).