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Method for separating and purifying zeaxanthin from marigold oleoresin

A technology for the separation and purification of zeaxanthin, which is applied in the direction of organic chemistry, can solve the problems of raw material waste cost, increase, and unsatisfactory yield, and achieve the effect of improving purity, high purity, and speeding up the resolution rate

Active Publication Date: 2019-12-13
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

However, there must be a loss of zeaxanthin in each separation process, which in turn leads to unsatisfactory yields, resulting in waste of raw materials and increased costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]1) Mix marigold oleoresin with ethyl acetate-ethanol solution (ethyl acetate:ethanol V / V, 6.5:1) at a mass ratio of 1:7, stir and dissolve; then transfer to a 6 kg macropore In the analysis column of the adsorption resin, the adsorption flow rate is 2BV / h, and the temperature is 50°C; after the adsorption is completed, rinse with deionized water until it is colorless; use ethyl acetate-ethanol analysis solution (ethyl acetate:ethanol V / V, 6.5:1 ) for analysis (marigold oleoresin: ethyl acetate-ethanol analysis solution w / w, 1:5), the analysis flow rate is 1BV / h, and the zeaxanthin analysis solution is collected;

[0035] 2) Concentrate the zeaxanthin ester analysis solution to obtain zeaxanthin ester extract; the residual volatiles in the zeaxanthin ester extract are controlled at 8% w / w;

[0036] 3) Hydrolyze zeaxanthin extract, propylene glycol, and 45% w / w potassium hydroxide aqueous solution (w / w, 1:0.5:0.7) in a reactor filled with carbon dioxide, and the temperatur...

Embodiment 2

[0040] 1) Mix marigold oleoresin with ethyl acetate-ethanol solution (ethyl acetate:ethanol V / V, 6:1) at a mass ratio of 1:8, stir and dissolve; then transfer to a 6 kg macropore In the analytical column of the adsorption resin, the adsorption flow rate is 1.5BV / h, and the temperature is 50°C; after the adsorption is completed, rinse with deionized water until it is colorless; use ethyl acetate-ethanol analysis solution (ethyl acetate: ethanol V / V, 6: 1) Perform analysis (marigold oleoresin: ethyl acetate-ethanol analysis solution w / w, 1:6), analysis flow rate 0.8BV / h, and collect zeaxanthin analysis solution;

[0041] 2) Concentrate the zeaxanthin ester analysis solution to obtain zeaxanthin ester extract; the residual volatile matter in the zeaxanthin ester extract is controlled at 6% w / w;

[0042] 3) The zeaxanthin extract, propylene glycol, and 40% w / w sodium hydroxide aqueous solution (w / w, 1:0.7:0.4) were hydrolyzed in a reactor filled with carbon dioxide, and the temper...

Embodiment 3

[0046] 1) Mix and dissolve marigold oleoresin and ethyl acetate-ethanol solution (ethyl acetate:ethanol V / V, 7:1) at a mass ratio of 1:6; In the analysis column of the resin, the adsorption flow rate is 2.5BV / h, and the temperature is 53°C; after the adsorption is completed, rinse with deionized water until it is colorless; use ethyl acetate-ethanol analysis solution (ethyl acetate:ethanol V / V, 7:1 ) for analysis (marigold oleoresin: ethyl acetate-ethanol analysis solution w / w, 1:4), the analysis flow rate is 1BV / h, and the zeaxanthin analysis solution is collected;

[0047] 2) Concentrate the zeaxanthin ester analysis solution to obtain zeaxanthin ester extract; the residual volatiles in the zeaxanthin ester extract are controlled at 5% w / w;

[0048] 3) Hydrolyze zeaxanthin extract, butanol, and 50% w / w potassium hydroxide aqueous solution (w / w, 1:0.3:0.8) in a reactor filled with carbon dioxide, and the temperature of the hydrolysis reaction is 80°C, the hydrolysis reaction...

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PUM

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Abstract

The invention discloses a method for separating and purifying zeaxanthin from marigold oleoresin, belonging to the technical field of extraction of natural effective components. The method is characterized by comprising the following steps: mixing marigold oleoresin with an ethyl acetate-ethanol dissolving solution according to a mass ratio of 1: (4-10), and carrying out dissolving; then transferring a formed solution into a desorption column filled with macroporous adsorption resin, and carrying out desorption by utilizing an ethyl acetate-ethanol desorption solution in a volume ratio of (5-10): 1 to obtain a desorption solution containing zeaxanthin ester; and subjecting the desorption solution containing zeaxanthin ester to concentration, saponification, crystallization, and grindingand refining to finally obtain high-purity zeaxanthin. The zeaxanthin obtained by using the method for separating and purifying zeaxanthin from marigold oleoresin in the invention is natural zeaxanthin with a purity of 95% or above and a high yield; and the method is convenient for large-scale production.

Description

technical field [0001] The invention discloses a method for separating and purifying zeaxanthin 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] Zeaxanthin, with a molecular formula of C40H56O2 and a molecular weight of 566.88, belongs to isoprenoids, an oxygen-containing carotenoid, and is isomers with lutein. Zeaxanthin can be used as a health additive and coloring agent. Zeaxanthin can resist oxidation, relieve visual fatigue, and prevent age-related macular degeneration. The macular pigment ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/24
CPCC07C403/24
Inventor 刘温来李勇杜明花殷东东赵辰光
Owner 山东天音生物科技有限公司