A method for preparing zeaxanthin crystals from marigold oleoresin without waste water

A technology of zeaxanthin and no waste water, applied in the direction of organic chemistry, etc., to achieve the effect of high conversion rate and high unit content

Active Publication Date: 2020-05-12
GUANGZHOU LEADER BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to overcome the difficulties and defects of the prior art in terms of environmental protection, to provide a method that produces no waste water, has a high yield of products, can continue to utilize by-products, and can achieve higher purity without recrystallization treatment. Environmentally friendly and economical method for industrial production of high-content zeaxanthin suitable for the food industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 5kg of marigold oleoresin with a lutein content of 15.0wt%, heat to 80°C and stir to melt the oleoresin, while taking 1.25kg of potassium hydroxide and adding it to 2.1kg of ethylene glycol and heating to 100°C and stirring to dissolve; Slowly add anhydrous alcohol-alkali solution to the fluid marigold oleoresin, and after 20 minutes, keep the temperature at 110°C for 3 hours; A large number of crystals precipitated; filtered while it was hot, the filter cake was washed twice with 3L of absolute ethanol, the filtrate was combined to recover ethanol, and finally the filter cake was vacuum-dried at 60°C for 3 hours to obtain 0.68 kg of orange-red zeaxanthin crystals, and the saponified filtrate was adjusted by adding citric acid. After reaching neutrality, the ethanol is distilled and recovered to obtain a paste with good water solubility and continuous utilization.

[0026] The obtained zeaxanthin crystals detected by ultraviolet-visible spectrophotometer have a tot...

Embodiment 2

[0028] Take 20kg of marigold oleoresin with a lutein content of 16.0wt%, heat to 100°C and stir to melt the oleoresin, and at the same time take 3kg of sodium hydroxide and add it to 6kg of propylene glycol and heat to 110°C and stir to dissolve; Slowly add anhydrous alcohol-alkali solution to the chrysanthemum oleoresin, after 30 minutes, keep the temperature at 120°C for 2.5 hours; then lower the temperature of the above system to 70°C and keep it warm, add 35L of absolute ethanol at 60°C, a large amount of crystals will precipitate ; Filtrate while hot, wash the filter cake twice with 12L anhydrous isopropanol, combine the filtrates, and finally dry the filter cake under vacuum at 60°C for 3 hours to obtain 2.9 kg of orange-red zeaxanthin crystals, add an appropriate amount of lauric acid to the saponification filtrate to adjust the pH value , after distilling and recovering the ethanol, the residue obtains a paste with good water solubility and can be continuously utilized....

Embodiment 3

[0031] Take 50kg of marigold oleoresin with a lutein content of 16.0wt%, heat to 100°C and stir to melt the oleoresin, and simultaneously add 12.5kg of sodium hydroxide to 21kg of propylene glycol and heat to 120°C and stir to dissolve; Slowly add anhydrous alcohol-alkali solution to marigold oleoresin, after 30 minutes, keep the temperature at 130°C for 3 hours; then cool down the above system to 70°C for heat preservation, add 100L of absolute ethanol at 60°C, a large number of crystals will precipitate ; Filtrate while hot, wash the filter cake twice with 30L absolute ethanol, combine the filtrates, and finally dry the filter cake under vacuum at 60°C for 3 hours to obtain 7.5kg of orange-red zeaxanthin crystals, add phosphoric acid to the saponification filtrate to neutralize, and recover by distillation The residue after ethanol gives a good water-soluble, reusable paste.

[0032] The obtained zeaxanthin crystals detected by the ultraviolet-visible spectrophotometer have ...

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PUM

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Abstract

In an existing preparation of zeaxanthin crystals, a large amount of alkaline colored waste water is produced in a washing and purification stage, the cost of environmental treatment is high, and environmental pollution is caused by emissions. The invention discloses a production process of finally preparing zeaxanthin crystals from marigold oil resin without waste water through a series of processes. The preparation method of the zeaxanthin crystals from the marigold oil resin without waste water is characterized in that the preparation method includes the steps of taking the marigold oil resin as raw material to be heated to a certain temperature in anhydrous or slightly watery conditions so that lutein esters are saponified in alcoholic solution of alkali and finally isomerized to zeaxanthin, using low-boiling anhydrous or low water content alcohol to wash saponification mixture, and recovering most alcohol solvent through vacuum distillation after the collection of the lotion; thesolvent can be reusable, remaining solid dry matter can be used directly as feed additives, and the cleanly-wasted zeaxanthin crystals can be used as food additives raw material without recrystallization.

Description

technical field [0001] The invention relates to a method for preparing zeaxanthin crystals, in particular to a method for preparing zeaxanthin crystals by saponifying marigold oleoresin without wastewater discharge. Background technique [0002] Zeaxanthin (Zeaxanthin, 3,3'-dihydroxy-β-carotene), is a polyene compound containing 9 alternating conjugated double bonds, one at each end of its carbon skeleton An ionone ring containing a hydroxyl group. Since zeaxanthin and lutein belong to a pair of isomers, their only difference lies in the distribution of the double bond position in the ionone ring, so the two often exist at the same time in natural plants. There are also many carotenoids in human blood, but studies have found that only zeaxanthin and lutein are concentrated in the central part of the retina in the inner part of the human eye, and play an important role in preventing age-related macular degeneration (AMD). Because the human body cannot synthesize zeaxanthin ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C403/24
CPCC07C403/24
Inventor 冼啟志林劲冬黄俊霖陶正国
Owner GUANGZHOU LEADER BIO TECH
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