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A method for separating and purifying lutein from marigold oleoresin

A technology for separation and purification of lutein, applied in the direction of organic chemistry, can solve the problems of low lutein yield, low lutein purity, and affecting purity, and achieve the goal of expanding the separation trend, accelerating the resolution rate, and high purity Effect

Active Publication Date: 2021-07-13
山东天音生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The applicant found the following problems in the research: first, the existing lutein extraction method has low purity of the obtained lutein, and contains a certain proportion of zeaxanthin in the lutein; the existing extraction method is to directly extract marigold oleoresin The lutein obtained by saponification will contain more zeaxanthin, and the proportion of zeaxanthin is 3%~9%, resulting in insufficient purity of lutein and waste of zeaxanthin; zeaxanthin is the The isomers of lutein need to add another separation process to remove zeaxanthin, and the increase of separation process will cause the loss of lutein
Second, the existing saponified lutein contains more salt impurities that are difficult to remove. These salt impurities are doped in the lutein crystals, which are difficult to remove and affect the purity.
The 3rd, the obtained lutein yield of existing method is low, causes the waste of raw material and the raising of production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Dissolve marigold oleoresin in ethyl acetate (marigold oleoresin:ethyl acetate w / w, 1:7); h, temperature 50°C; after adsorption is complete, rinse with deionized water until colorless; add ethyl acetate-ethanol analysis solution (V / V, 6.5:1) for analysis (Marigold oleoresin: ethyl acetate-ethanol analysis solution w / w, 1:5), the analysis flow rate is 1.5BV / h, using the n-hexane-ethyl acetate mixture as the analysis solution for analysis, and the analysis solution is obtained to obtain the lutein ester analysis solution;

[0036] 2) Concentrate the lutein ester analysis solution under reduced pressure and recover the solvent to obtain the lutein ester extract; the residual volatiles in the lutein ester extract are controlled at 7% w / w;

[0037] 3) The lutein ester extract, propylene glycol, potassium hydroxide aqueous solution and vitamin E are hydrolyzed in a reaction kettle fed with carbon dioxide. The temperature of the hydrolysis reaction is 60°C, and the hydrolys...

Embodiment 2

[0041]1) Dissolve marigold oleoresin in ethyl acetate (marigold oleoresin: ethyl acetate w / w, 1:6); then transfer it to an analytical column filled with 16 kg of 200 mesh silica gel, and the adsorption flow rate is 1.5BV / h, temperature 50°C; after adsorption is complete, rinse with deionized water until colorless; add ethyl acetate-ethanol analysis solution (V / V, 7:1) for analysis (marigold oleoresin: ethyl acetate-ethanol analysis Liquid w / w, 1:4), analysis flow rate 1.5BV / h, use n-hexane-ethyl acetate mixture as analysis solution for analysis, and analyze to obtain lutein ester analysis solution;

[0042] 2) Concentrate the lutein ester analysis solution and recover the solvent to obtain the lutein ester extract; the residual volatile matter in the lutein ester extract is controlled at 8% w / w;

[0043] 3) The lutein ester extract, glycerol, sodium hydroxide aqueous solution and vitamin E are hydrolyzed in a reaction kettle filled with carbon dioxide. The temperature of the ...

Embodiment 3

[0047] 1) Dissolve marigold oleoresin in ethyl acetate (marigold oleoresin: ethyl acetate w / w, 1:8); then transfer it to an analytical column filled with 60 kg of 100 mesh silica gel, and the adsorption flow rate is 1.5BV / h, temperature 50°C; after adsorption is complete, rinse with deionized water until colorless; add ethyl acetate-ethanol analysis solution (V / V, 6:1) for analysis (marigold oleoresin: ethyl acetate-ethanol analysis liquid w / w, 1:6), the analysis flow rate is 0.5BV / h, and the analysis is carried out by using n-hexane-ethyl acetate mixture as the analysis solution, and the analysis solution is obtained by analysis of lutein ester;

[0048] 2) Concentrate the lutein ester analysis solution and recover the solvent to obtain the lutein ester extract; the residual volatile matter in the lutein ester extract is controlled at 6% w / w;

[0049] 3) The lutein ester extract, butanol, potassium hydroxide aqueous solution and vitamin E are hydrolyzed in a reaction kettle ...

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Abstract

The invention discloses a method for separating and purifying lutein from marigold oleoresin, which belongs to the technical field of extraction of natural active ingredients. It is characterized in that, the preparation steps are: dissolving marigold oleoresin in ethyl acetate, then using n-hexane-ethyl acetate mixture solution for analysis, analysis to obtain lutein ester analysis solution, and concentrating to obtain lutein ester extract; The lutein ester extract is hydrolyzed with alcohol, lye and antioxidants in a reactor fed with carbon dioxide; the lutein saponified product is diluted with ethanol, allowed to stand, and filtered to obtain crude lutein crystals; wet , grinding and crushing, dissolving, filtering and drying to obtain lutein crystals. This product hardly contains other carotenoids such as zeaxanthin, is a pure natural product, and is convenient for large-scale production.

Description

technical field [0001] The invention discloses a method for separating and purifying lutein from marigold oleoresin, which belongs to the technical field of extraction of natural active ingredients. Background technique [0002] Marigold oleoresin is a yellow or brown solid or viscous liquid, which is extracted from the dried flowers of the Compositae plant marigold (usually protected from light), after drying and crushing, with an organic solvent (usually n-hexane) , and then volatilize to remove the solvent, and the obtained extract is marigold oleoresin, and the marigold oleoresin contains carotenoid ester. [0003] Lutein is a carotenoid with good antioxidant properties, and has unique functions in relieving visual fatigue, preventing age-related macular degeneration, protecting skin, enhancing immunity and reducing the incidence of cardiovascular diseases. Lutein has health care and coloring functions. One prepared source of lutein is extracted from marigold flowers. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C403/24
CPCC07C403/24C07C2601/16
Inventor 刘温来李勇殷东东赵辰光田芸
Owner 山东天音生物科技有限公司