CN104447460A - Xanthophyll preparation technology - Google Patents
Xanthophyll preparation technology Download PDFInfo
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- CN104447460A CN104447460A CN201310431306.8A CN201310431306A CN104447460A CN 104447460 A CN104447460 A CN 104447460A CN 201310431306 A CN201310431306 A CN 201310431306A CN 104447460 A CN104447460 A CN 104447460A
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- xenthophylls
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Abstract
A xanthophyll preparation technology adopting marigold oil as a raw material comprises the following steps: 1, adding marigold oil into an aqueous glycerol solution containing calcium hydroxide, uniformly stirring, and reacting at 30-65DEG C under light-resistant nitrogen protection conditions; 2, filtering the obtained reaction mixture, collecting filter residues, washing with hot water until neutrality, washing the filter residues with an organic solvent until the obtained filtrate is colorless, collecting the organic solvent filtrate, and carrying out reduced pressure concentration at 30-45DEG C to obtain crude xanthophylls; and 3, washing the crude xanthophyll with anhydrous ethanol, and carrying out vacuum drying to obtain a xanthophyll product. The technology has the advantages of simplicity, low cost and environmental protection, and the obtained xanthophyll is highly pure, and is suitable for industrial scale production.
Description
Technical field
The invention belongs to natural pigment preparation field, be specifically related to a kind of xenthophylls preparation technology.
Background technology
Xenthophylls is a kind of natural pigment, has the feature of lovely luster, strong coloring force, safety non-toxic, antioxidant property excellence, has been widely used in the production fields such as food, makeup, tobacco, animal and fowl fodder.Scientific research in recent years report xenthophylls with reduce cause the danger of age related macular degeneration (AMD) relevant by oxidative damage macula retinae district, and xenthophylls can effectively prevention of arterial harden, cataract, also can suppress the generation of cancer.A large amount of xenthophylls is present in vegetables, flowers, fruit and some algae bio, wherein especially the highest with content in mary bush and Flower of Aztec Marigold.Xenthophylls in plant usually and the lipid acid such as tetradecanoic acid, lauric acid and palmitinic acid be combined into ester derivative, but lutein ester need change into free xenthophylls can by body metabolism, therefore from needing hydrolysis containing the lutein ester prepared the biology of xenthophylls, free xenthophylls monomer is generated.Current method for hydrolysis is chemical reagent saponification method and esterase solution mainly.Chemical reagent saponification method uses inorganic strong alkali usually, and corrodibility is strong, and emulsion is comparatively serious, is unfavorable for that the later stage is separated.Esterase solution can solve the chemical residue problem of traditional chemical reagent saponification method, but enzyme digestion reaction cost is high, and the problem that enzymolysis not exclusively can cause quality product to reduce, and above generally still selects chemical reagent saponification method so produce.
Summary of the invention
The object of the invention is the defect overcoming original xenthophylls preparation method, providing a kind of is raw material with marigold oil resin, and work simplification, cost are low, meets environmental requirement and is suitable for the preparation method of xenthophylls of commercial scale production.
To achieve these goals, the present invention is raw material with marigold oil resin, comprises the steps:
(1) marigold oil resin is joined in the aqueous glycerin solution of calcium hydroxide, stir, under lucifuge and nitrogen protection, react at 30 ~ 65 DEG C;
(2) filter reaction mixture, collect filter residue, hot wash is to neutral rear colourless to filtrate with organic solvent washing filter residue, and collect organic solvent filtrate, 30 ~ 45 DEG C of concentrating under reduced pressure obtain xenthophylls crude product;
(3) absolute alcohol washing xenthophylls crude product, obtains xenthophylls product through vacuum-drying.
Wherein, in the aqueous glycerin solution of the middle calcium hydroxide of step (1), aqueous glycerin solution mass concentration 80 ~ 95%, the consumption of calcium hydroxide is 0.03 ~ 0.06 grams per milliliter aqueous glycerin solution; Marigold oil resin charging capacity is 0.10 ~ 0.12 grams per milliliter aqueous glycerin solution; Reaction times is 12 ~ 24 hours.
Wherein in step (2), hot water temperature is 50 ~ 65 DEG C, and described organic solvent is ethyl acetate, acetone or tetrahydrofuran (THF).
Wherein in step (3), absolute alcohol is anhydrous methanol, dehydrated alcohol, anhydrous isopropyl alcohol.
Advantage of the present invention is as follows:
1. work simplification, cost be low, be suitable for commercial scale production.
2. it is even nontoxic that the solvent that preparation process is selected is low toxicity, meets environmental requirement.
3. the purity of xenthophylls product can reach 90%.
4, embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
A kind of xenthophylls preparation technology, is raw material with marigold oil resin, comprises the steps:
(1) marigold oil resin is joined in the aqueous glycerin solution of calcium hydroxide, stir, under lucifuge and nitrogen protection, react at 30 ~ 65 DEG C;
(2) filter reaction mixture, collect filter residue, hot wash is to neutral rear colourless to filtrate with organic solvent washing filter residue, and collect organic solvent filtrate, 30 ~ 45 DEG C of concentrating under reduced pressure obtain xenthophylls crude product;
(3) absolute alcohol washing xenthophylls crude product, obtains xenthophylls product through vacuum-drying.
Wherein, in the aqueous glycerin solution of the middle calcium hydroxide of described step (1), aqueous glycerin solution mass concentration 80 ~ 95%, the consumption of calcium hydroxide is 0.03 ~ 0.06 grams per milliliter aqueous glycerin solution; Marigold oil resin charging capacity is 0.10 ~ 0.12 grams per milliliter aqueous glycerin solution; Reaction times is 12 ~ 24 hours.
In described step (2), hot water temperature is 50 ~ 65 DEG C, and described organic solvent is ethyl acetate, acetone or tetrahydrofuran (THF).
In described step (3), absolute alcohol is anhydrous methanol, dehydrated alcohol, anhydrous isopropyl alcohol.
Example 1
It is in the aqueous glycerin solution of 95% that 15 grams of calcium hydroxides are scattered in 500 milliliters of mass concentrations, adds 50 grams of marigold oil resins, stirs.Under lucifuge and nitrogen protection; react 12 hours at 65 DEG C; reaction mixture is filtered; collect filter residue; first with the hot wash filter residue of 50 DEG C to washings in neutral; then colourless to filtrate with ethyl acetate washing filter residue, collect ethyl acetate filtrate, 30 DEG C of concentrating under reduced pressure obtain xenthophylls crude product 4.3 grams.With the xenthophylls crude product of 430 milliliters of absolute ethanol washing gained, vacuum-drying obtains xenthophylls product 3.2 grams in 24 hours, and purity is 90.7%
Example 2
It is in the aqueous glycerin solution of 80% that 30 grams of calcium hydroxides are scattered in 500 milliliters of mass concentrations, adds 60 grams of marigold oil resins and stirs.Under lucifuge and nitrogen protection; react 18 hours at 30 DEG C; reaction mixture is filtered; collect filter residue; first with the hot wash filter residue of 65 DEG C to washings in neutral; then use washing with acetone filter residue colourless to filtrate, collect acetone filtrate, at 30 DEG C, concentrating under reduced pressure obtains xenthophylls crude product 6.0 grams.With the xenthophylls crude product of 300 milliliters of anhydrous isopropyl alcohol washing gained, vacuum-drying obtains xenthophylls product 4.8 grams in 24 hours, and purity is 87.4%.
Example 3
It is in the aqueous glycerin solution of 90% that 20 grams of calcium hydroxides are scattered in 500 milliliters of mass concentrations, adds 55 grams of marigold oil resins, stirs.Under lucifuge and nitrogen protection; react 20 hours at 40 DEG C; reaction mixture is filtered; collect filter residue; first with the hot wash filter residue of 60 DEG C to washings in neutral; then colourless to filtrate with tetrahydrofuran (THF) washing filter residue, collect tetrahydrofuran (THF) filtrate, 40 DEG C of concentrating under reduced pressure obtain xenthophylls crude product 5.3 grams.With the xenthophylls crude product of 430 milliliters of absolute ethanol washing gained, vacuum-drying obtains xenthophylls product 4.8 grams in 24 hours, and purity is 90%.
Example 4
It is in the aqueous glycerin solution of 85% that 25 grams of calcium hydroxides are scattered in 500 milliliters of mass concentrations, adds 50 grams of marigold oil resins, stirs.Under lucifuge and nitrogen protection; react 18 hours at 60 DEG C; reaction mixture is filtered; collect filter residue; first with the hot wash filter residue of 60 DEG C to washings in neutral; then colourless to filtrate with ethyl acetate washing filter residue, collect ethyl acetate filtrate, 40 DEG C of concentrating under reduced pressure obtain xenthophylls crude product 5.0 grams.With the xenthophylls crude product of 500 milliliters of absolute ethanol washing gained, vacuum-drying obtains xenthophylls product 3.8 grams in 24 hours, and purity is 90.2%.
Claims (6)
1. an xenthophylls preparation technology, is characterized in that: be raw material with marigold oil resin, comprises the steps:
(1) marigold oil resin is joined in the aqueous glycerin solution of calcium hydroxide, stir, under lucifuge and nitrogen protection, react at 30 ~ 65 DEG C;
(2) filter reaction mixture, collect filter residue, hot wash is to neutral rear colourless to filtrate with organic solvent washing filter residue, and collect organic solvent filtrate, 30 ~ 45 DEG C of concentrating under reduced pressure obtain xenthophylls crude product;
(3) absolute alcohol washing xenthophylls crude product, obtains xenthophylls product through vacuum-drying.
2. according to the preparation method of the xenthophylls described in claim 1, it is characterized in that: in the aqueous glycerin solution of the calcium hydroxide described in step (1), aqueous glycerin solution mass concentration 80 ~ 95%, the consumption of calcium hydroxide is 0.03 ~ 0.06 grams per milliliter aqueous glycerin solution.
3. according to the preparation method of the xenthophylls described in claim 1, it is characterized in that: the marigold oil resin charging capacity described in step (1) is 0.10 ~ 0.12 grams per milliliter aqueous glycerin solution.
4. according to the preparation method of the xenthophylls described in claim 1, it is characterized in that: the reaction times described in step (1) is 12 ~ 24 hours.
5. according to the preparation method of the xenthophylls described in claim 1, it is characterized in that: the hot water temperature described in step (2) is 50 ~ 65 DEG C, described organic solvent is ethyl acetate, acetone or tetrahydrofuran (THF).
6. according to the preparation method of the xenthophylls described in claim 1, it is characterized in that: the absolute alcohol described in step (3) is anhydrous methanol, dehydrated alcohol, anhydrous isopropyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310431306.8A CN104447460A (en) | 2013-09-22 | 2013-09-22 | Xanthophyll preparation technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310431306.8A CN104447460A (en) | 2013-09-22 | 2013-09-22 | Xanthophyll preparation technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104447460A true CN104447460A (en) | 2015-03-25 |
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| CN201310431306.8A Pending CN104447460A (en) | 2013-09-22 | 2013-09-22 | Xanthophyll preparation technology |
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| CN (1) | CN104447460A (en) |
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- 2013-09-22 CN CN201310431306.8A patent/CN104447460A/en active Pending
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Application publication date: 20150325 |