CN104432003A - High-purity lutein ester composition and preparation process thereof - Google Patents

High-purity lutein ester composition and preparation process thereof Download PDF

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Publication number
CN104432003A
CN104432003A CN201310431363.6A CN201310431363A CN104432003A CN 104432003 A CN104432003 A CN 104432003A CN 201310431363 A CN201310431363 A CN 201310431363A CN 104432003 A CN104432003 A CN 104432003A
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filter cake
lutein
filter
alcohol
product
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谭超智
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Qingdao Zhongren Zhiye Biological Technology Co Ltd
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Qingdao Zhongren Zhiye Biological Technology Co Ltd
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
    • A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
    • A23L5/273—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption using adsorption or absorption agents, resins, synthetic polymers, or ion exchangers
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
    • C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a high-purity lutein ester composition and a preparation process thereof. The preparation method comprises the following steps: cooling a solution of a solvent A of a marigold extract until the temperature is 20-30 DEG C, keeping for 0.5-4h, then cooling until the temperature is 5-20 DEG C, keeping for 0.5-4h, and filtering to obtain a filter cake I; under the condition with the temperature of 30-70 DEG C, dissolving the filter cake I in a mixed solvent A, stirring for 0.5-5h, cooling until the temperature is 10-28 DEG C, keeping for 0.5-5h, and filtering to obtain a filter cake II; and carrying out subsequent steps, wherein the mixed solvent A is prepared from methyl acetate, ethyl acetate, n-propyl acetate or butyl acetate and C1-3 alcohol. By virtue of the preparation method, the process is simple and feasible, and is easy in industrialization, all operations are carried out at low temperature, and the stability of the product is ensured; the product yield reaches up to above 25 percent, the total ester content of the product is larger than 70 percent, the trans-lutein content reaches up to 90-93 percent, and the biological activity of the product during application is greatly improved.

Description

A kind of high-purity lutein ester composition and preparation technology
Technical field
The method that the present invention relates to and be separated high-content lutein ester product from marigold extractum, especially there is the composition of high trans lutein ester content.Particularly relate to the method utilizing direct crystallization method to obtain the said goods.
 
Background technology
Lutein ester is a kind of carotenoid fatty acid ester existed with aliphatic acid and lutein combining form.It is extensively present in the plants such as pumpkin, spinach, wild cabbage, marigold flower.Research shows, takes in lutein ester and can improve lutein levels in blood and macula retinae, thus prevention age related is looked yellow class and degenerated and cataract, and can effectively grow and the generation of atherosclerosis by Tumor suppression.Lutein and zeaxanthin are the carotenoid being uniquely present in human retina macular area, and human body self can not be synthesized lutein and must be supplemented it by ordinary meal.The lutein ester of occurring in nature has two kinds of configurations, is trans and cis respectively, wherein based on alltrans molecular configuration.Alltrans lutein ester can be divided into again: lutein monoesters and lutein diester.
In the plants such as marigold, free lutein content is less, and mostly by modifications such as laurate, myristic acid, palmitic acids, the ester that wherein content is the highest is lutein palmitic acid diester (A Subagio NMorita.Food Reasearchinternation, 2001,34: 315-320)
This technique provides a kind of preparation of high-purity lutein ester, stable state and method for removing pollutant thereof: first removed by the acetone insoluble matter in marigold extractum, carry out isopropyl alcohol or butanol crystallizing with the concentrate of imurity-removal again, finally use lower alcohol washing crystal again.Wherein two-step crystallization solvent for use is different, there is certain solvent and intersects, isopropyl alcohol or the butanol crystallizing used time longer, be unfavorable for the lifting of production efficiency.There is a large amount of solvent with isopropyl alcohol or butanols and intersect in the washing of final step lower alcohol, and the product yield of the method is very low, only has 11 ~ 15%.The present invention has used for reference the wherein method of pollutant removing and antioxidant interpolation, but has carried out substantial improvement to the crystallization processes of core in this technical scheme.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of safe, convenient, high-purity lutein ester product that product yield is high and corresponding lutein ester product.
The preparation method of the composition containing lutein ester of the present invention, comprises the steps:
A. under 30 ~ 70 DEG C of conditions, marigold extractum is dissolved in mixed solvent A, adds adsorbent and stir 0.5 ~ 5 hour, filter, collect filtrate;
B. the filtrate of step a is cooled to 20 ~ 28 DEG C, keeps after 0.5 ~ 4 hour, then be cooled to 5 ~ 18 DEG C and keep 0.5 ~ 4 hour, filter to obtain filter cake I;
C., under 30 ~ 70 DEG C of conditions, dissolving filter cake I, in mixed solvent A, stirs and is cooled to 10 ~ 28 DEG C after 0.5 ~ 5 hour and keeps 0.5 ~ 5 hour, filter to obtain filter cake II;
D. use C1-3 alcohol washing leaching cake II, then add antioxidant, then the C1-3 alcohol that dry removing is residual, obtain the composition containing lutein ester;
Wherein said mixed solvent A is the mixed solvent of methyl acetate, ethyl acetate, n-propyl acetate or butyl acetate and C1-3 alcohol.
Marigold extractum of the present invention is the medicinal extract that marigold flower grain obtains through organic solvent extraction, and wherein total ester mass percentage should be 18 ~ 35%.The organic solvent of normal use is propane or No. six solvents (GB16629-19966 solvent for extraction).
C1-3 alcohol of the present invention refers to methyl alcohol, ethanol, propyl alcohol or isopropyl alcohol.
In the preferred technical scheme of this law, the mixed solvent A in described method is the binary mixed solvent of methyl acetate/methyl alcohol, ethyl acetate/ethanol or n-propyl acetate/isopropyl alcohol.Most preferably the mixed solvent of methyl acetate/methyl alcohol or ethyl acetate/ethanol.
In the method for the invention described above, in described mixed solvent A, the mass ratio of ester and alcohol is 2: 8 ~ 9: 1.
In another optimal technical scheme of the present invention, the mass ratio of the marigold extractum in described step a and mixed solvent A is 1: 0.5 ~ 1: 20, preferably 1: 0.5 ~ 1: 15, most preferably 1: 1 ~ 1: 10; In step c, the mass ratio of filter cake I and mixed solvent A is 1: 0.5 ~ 20, preferably 1: 0.5 ~ 1: 15, most preferably 1: 1 ~ 1: 10.
In another optimal technical scheme of the present invention, described step b and the rate of temperature fall of step c are 5 ~ 20 DEG C/h, more preferably 5 ~ 15 DEG C/h.
In an optimal technical scheme more of the present invention, the alcohol in described steps d is ethanol or isopropyl alcohol, preferred alcohol; The consumption of alcohol is 3 ~ 30 times of filter cake II quality, preferably 3 ~ 20 times, most preferably 4 ~ 15 times.
In arbitrary technical scheme of the invention described above, the adsorbent addressed is selected from the mixture that active carbon, carclazyte, diatomite, EDTA, EDTA disodium salt and two or more adsorbent above-mentioned form with arbitrary proportion; Preferably with the mixture that in active carbon, carclazyte, diatomite, 1 ~ 3 kind forms with arbitrary proportion; Most preferably active carbon, diatomite or the two with arbitrary proportion composition mixture.Wherein said active carbon is with shell and wood chip for raw material, through charing, activation, refiningly to process; Diatomite mainly more than 90% diatom test composition.
In arbitrary technical scheme of the invention described above, the antioxidant in described steps d is selected from the mixture that vitamin E, Vc sodium, sodium isoascorbate, Vc palmitate, Tea Polyphenols and two or more antioxidant above-mentioned mix with arbitrary proportion; Preferred vitamin E, different Vc sodium, Vc palmitate or Tea Polyphenols and two or more antioxygen above-mentioned
The mixture that agent mixes with arbitrary proportion; Most preferably vitamin E, Vc palmitate or mixture that the two mixes with arbitrary proportion.
In the further optimal technical scheme of the present invention, baking temperature 30 ~ 70 DEG C in described steps d, be dried to molten residual≤1ppm.
Another preferred technical scheme of the present invention is omnidistance N2 gas shielded in whole preparation process.
The object of another aspect of the present invention is to provide the composition containing lutein ester prepared by said method.
Use said method of the present invention to prepare containing the composition of lutein ester, whole simple for process, be easy to industrialization,
All operations carries out all at low temperatures, ensure that the stability of product to the full extent.Products obtained therefrom yield is high, and weight yield can reach more than 25%, and can also ensure that the total ester content of product is greater than 70% while guarantee yield, and trans-lutein content, up to 90 ~ 93%, improves biologically active when product uses greatly.
Adsorbent selected in addition can remove heavy metal and pesticide remnant residual in marigold extractum effectively, and mixed solvent also has the effect removing harmful substance, thus ensure that the high-quality of the lutein ester product finally obtained.Antioxidant is added after low-carbon alcohols kind solvent washing leaching cake, lutein ester product can be prevented oxidized in drying course, experiment proves to add appropriate antioxidant in lutein ester product, can ensure that it is under room temperature in vacuo terms of packing, never degenerates in 3 years.And solvent for use of the present invention is food grade solvent, the product prepared meets food sanitation safe.
4, detailed description of the invention
The active carbon adopted in the present invention meets GB/T 13803.4-1999 standard; Carclazyte meets GB25571-2010 standard, and diatomite meets GB 24265-2009 standard.
The present invention uses method measuring and calculating lutein ester total ester content disclosed in JP 2003201497 (A); AOAC Offical Method 970.64 (Carotenes and Xanthophylls in Dried PlantMaterialsand Mixed Feeds) is used to measure content and the composition of alltrans lutein and alltrans zeaxanthin in lutein ester.
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Wherein said " total ester content " is lutein ester total ester content, according to mass percent.
Embodiment 1
Take the marigold extractum that 100g total ester content is 28wt%, mix with methyl acetate/methyl alcohol (weight ratio is 2: 8) 1100g, add 7g diatomite and at 60 DEG C, add thermal agitation filter after 3.5 hours, obtain mother liquor I.Mother liquor I is kept 3h after 1h is cooled to 27 DEG C, then is cooled to 9 DEG C through 1h and keeps filtering after 4h obtaining filter cake I.
Methyl acetate/methyl alcohol (weight ratio is 2: 8) the dissolving filter cake I of filter cake I quality 4 times is added at 55 DEG C, filter after slow cooling to 11 DEG C keeps 3.5h after adding thermal agitation 5h and obtain filter cake II, add the methyl alcohol agitator treating filter cake II of its quality 12 times, 1.2g Tea Polyphenols and 0.6g vitamin C is added in solid after methanol wash, 5h is dried at 45 DEG C, obtain product 27g, mass percentage after testing containing lutein ester is 67%, wherein alltrans lutein: zeaxanthin (mol ratio)=91: 5.
Embodiment 2
Taking 100g total ester content is that the marigold extractum of 27wt % mixes with methyl acetate/ethanol (weight ratio is 2.5: 7.5) 1800g, adds 6.5gEDTA and 0.5g carclazyte and at 48 DEG C, adds thermal agitation filter after 3 hours, obtain mother liquor I.Mother liquor I slow cooling is kept 1h after 1h is cooled to 23.5 DEG C, then is cooled to 13 DEG C through 1h and keeps filtering after 2.5h obtaining filter cake I.
Methyl acetate/isopropyl alcohol (weight ratio is 5: 5) the dissolving filter cake I of filter cake I quality 0.5 times is added at 60 DEG C, filter after slow cooling to 11.5 DEG C keeps 4h after adding thermal agitation 2h and obtain filter cake II, add the methyl alcohol agitator treating filter cake II of its quality 8 times, add 0.5g vitamin E and 0.3g Vc palmitate in solid after methanol wash, dry at 32 DEG C
Dry 17h, obtains product 26g, and the mass percentage after testing containing lutein ester is 66%, wherein alltrans lutein: zeaxanthin (mol ratio)=91: 6.
Embodiment 3
Taking 100g total ester content is that the marigold extractum of 26wt % mixes with ethyl acetate/methyl alcohol (weight ratio is 2: 8) 1350g, adds 15g carclazyte and at 32 DEG C, adds thermal agitation filter after 4.5 hours, obtain mother liquor I.Mother liquor I slow cooling is kept 3h after 1h is cooled to 26.5 DEG C, then is cooled to 8.5 DEG C through 1h and keeps filtering after 1.5h obtaining filter cake I.
Ethyl acetate/isopropyl alcohol (weight ratio is 6: 4) the dissolving filter cake I of filter cake I quality 20 times is added at 65 DEG C, filter after slow cooling to 28 DEG C keeps 1h after adding thermal agitation 0.5h and obtain filter cake II, add the isopropyl alcohol agitator treating filter cake II of its quality 30 times, 1.5g vitamin E is added in solid after washed with isopropyl alcohol, 24h is dried at 30 DEG C, obtain product 20g, mass percentage after testing containing lutein ester is 70%, wherein alltrans lutein: zeaxanthin (mol ratio)=91 6.
Embodiment 4
Taking 100g total ester content is that the marigold extractum of 28wt% mixes with n-propyl acetate/propyl alcohol (weight ratio is 3: 7) 800g, adds 3g active carbon and 2g EDTA and at 40 DEG C, adds thermal agitation filter after 3 hours, obtain mother liquor I.
Mother liquor I slow cooling is kept 4h after 40min is cooled to 28 DEG C, then is cooled to 18 DEG C through 40min and keeps filtering after 4h obtaining filter cake I.
N-propyl acetate/propyl alcohol (weight ratio is 3: 7) the dissolving filter cake I of filter cake I quality 8 times is added at 60 DEG C, filter after slow cooling to 10 DEG C keeps 0.5h after adding thermal agitation 2.5h and obtain filter cake II, add the isopropyl alcohol agitator treating filter cake II of its quality 10 times, 1.2g vitamin C palmitate and 0.6g sodium isoascorbate is added in solid after washed with isopropyl alcohol, 1h is dried at 50 DEG C, obtain product 24g, mass percentage after testing containing lutein ester is 71%, wherein alltrans lutein: zeaxanthin (mol ratio)=90: 5.
Embodiment 5
Taking 100g total ester content is that the marigold extractum of 28wt % mixes with ethyl acetate/ethanol (weight ratio is 3: 7) 1000g, adds 7g diatomite and 1g carclazyte and at 30 DEG C, adds thermal agitation filter after 5 hours, obtain mother liquor I.
Mother liquor I slow cooling is kept 4h after 40min is cooled to 20 DEG C, then is cooled to 11 DEG C through 40min and keeps filtering after 4h obtaining filter cake I.
Ethyl acetate/ethanol (weight ratio is 3: 7) the dissolving filter cake I of filter cake I quality 1 times is added at 30 DEG C, filter after slow cooling to 10 DEG C keeps 0.5h after adding thermal agitation 5h and obtain filter cake II, add the isopropyl alcohol agitator treating filter cake II of its quality 3 times, the different Vc sodium of 1g is added in solid after washed with isopropyl alcohol, 3h is dried at 70 DEG C, obtain product 26g, mass percentage after testing containing lutein ester is 68%, wherein alltrans lutein: zeaxanthin (mol ratio)=92: 6.
Embodiment 6
Taking 100g total ester content is that the marigold extractum of 26wt% mixes with n-propyl acetate/isopropyl alcohol (weight ratio is 3: 7) 2000g, adds 3g carclazyte and 7gEDTA and at 38 DEG C, adds thermal agitation filter after 4.5 hours, obtain mother liquor I.Mother liquor I slow cooling is kept 4h after 40min is cooled to 27.5 DEG C, then is cooled to 6.5 DEG C through 40min and keeps filtering after 3h obtaining filter cake I.
N-propyl acetate/isopropyl alcohol (weight ratio is 3: 7) the dissolving filter cake I of filter cake I quality 12 times is added at 60 DEG C, filter after slow cooling to 25.5 DEG C keeps 2.5h after adding thermal agitation 4.5h and obtain filter cake II, add the methyl alcohol agitator treating filter cake II of its quality 30 times, 0.2g Tea Polyphenols and the different Vc sodium of 1g is added in solid after washed with isopropyl alcohol, 10h is dried at 44 DEG C, obtain product 22g, mass percentage after testing containing lutein ester is 70%, wherein alltrans lutein: zeaxanthin (mol ratio)=92: 6.
Embodiment 7
Taking 100g total ester content is that the marigold extractum of 27wt% mixes with butyl acetate/isopropyl alcohol (weight ratio is 4: 6) 1300g, adds 3gEDTA disodium salt and 4g diatomite and at 60 DEG C, adds thermal agitation filter after 1 hour, obtain mother liquor I.Mother liquor I slow cooling is kept 2h after 1h is cooled to 26 DEG C, then is cooled to 12 DEG C through 40min and keeps filtering after 2.5h obtaining filter cake I.
Butyl acetate/ethanol (weight ratio is 6: 4) the dissolving filter cake I of filter cake I quality 1 times is added at 45 DEG C, filter after slow cooling to 13 DEG C keeps 2h after adding thermal agitation 1.5h and obtain filter cake II, add the ethanol agitator treating filter cake II of its quality 20 times, 0.4g vitamin E and 1.4g vitamine C palmitate is added in solid after ethanol washing, 12h is dried at 40 DEG C, obtain product 28g, mass percentage after testing containing lutein ester is 67%, wherein alltrans lutein: zeaxanthin (mol ratio)=92: 5.
Embodiment 8
Taking 100g total ester content is that the marigold extractum of 27wt % mixes with methyl acetate/methyl alcohol (weight ratio is 4: 6) 100g, adds 2g carclazyte and 2g diatomite and at 45 DEG C, adds thermal agitation filter after 4 hours, obtain mother liquor I.Mother liquor I slow cooling is kept 0.5h after 40min is cooled to 21 DEG C, then is cooled to 7 DEG C through 1h and keeps filtering after 1h obtaining filter cake I.
Methyl acetate/methyl alcohol (weight ratio is 4: 6) the dissolving filter cake I of filter cake I matter 1 times is added at 55 DEG C, filter after slow cooling to 17 DEG C keeps 5h after adding thermal agitation 3h and obtain filter cake II, add the isopropyl alcohol agitator treating filter cake II of its quality 8 times, 0.4g Vc palmitate is added in solid after washed with isopropyl alcohol, 24h is dried at 30 DEG C, obtain product 26g, mass percentage after testing containing lutein ester is 72%, wherein alltrans lutein: zeaxanthin (mol ratio)=92: 5.
Embodiment 9
Taking 100g total ester content is that the marigold extractum of 27wt% mixes with n-propyl acetate/isopropyl alcohol (weight ratio is 4.5: 5.5) 1600g, adds 1g diatomite and 12g active carbon and at 65 DEG C, adds thermal agitation filter after 1.5 hours, obtain mother liquor I.Mother liquor I slow cooling is kept 1.5h after 1h is cooled to 25 DEG C, then is cooled to 6 DEG C through 1h and keeps filtering after 1h obtaining filter cake I.
N-propyl acetate/isopropyl alcohol (weight ratio is 4.5: 5.5) the dissolving filter cake I of filter cake I quality 17 times is added at 30 DEG C, filter after slow cooling to 14 DEG C keeps 3.5h after adding thermal agitation 4.5h and obtain filter cake II, add the isopropyl alcohol agitator treating filter cake II of its quality 8 times, 0.5g Vc palmitate and 1g vitamin C is added in solid after methanol wash, 11h is dried at 54 DEG C, obtain product 25g, mass percentage after testing containing lutein ester is 73%, wherein alltrans lutein: zeaxanthin (mol ratio)=91: 6.
Embodiment 10
Taking 100g total ester content is that the marigold extractum of 28wt% mixes with methyl acetate/ethanol (weight ratio is 5: 5) 1000g, adds 10g carclazyte and at 70 DEG C, adds thermal agitation filter after 0.5 hour, obtain mother liquor I.Mother liquor I slow cooling is kept 3h after 1h is cooled to 20 DEG C, then is cooled to 10 DEG C through 40min and keeps filtering after 1.5h obtaining filter cake I.
Methyl acetate/ethanol (weight ratio is 5: 5) the dissolving filter cake I of filter cake I quality 10 times is added at 60 DEG C, filter after slow cooling to 22 DEG C keeps 5h after adding thermal agitation 2h and obtain filter cake II, add the methyl alcohol agitator treating filter cake II of its quality 15 times, 0.5g vitamin C sodium salt is added in solid after methanol wash, 4h is dried at 70 DEG C, obtain product 26g
Mass percentage after testing containing lutein ester is 74%, wherein alltrans lutein: zeaxanthin (mol ratio)=93: 6.
Embodiment 11
Taking 100g total ester content is that the marigold extractum of 28wt % mixes with methyl acetate/methyl alcohol (weight ratio is 5: 5) 700g, adds 1g diatomite and 8gEDTA and at 70 DEG C, adds thermal agitation filter after 0.5 hour, obtain mother liquor I.Mother liquor I slow cooling is kept 3.5h after 1h is cooled to 23 DEG C, then is cooled to 13 DEG C through 40min and keeps filtering after 2h obtaining filter cake I.
Methyl acetate/methyl alcohol (weight ratio is 2: 8) the dissolving filter cake I of filter cake I quality 20 times is added at 70 DEG C, filter after slow cooling to 5.5 DEG C keeps 3.5h after adding thermal agitation 2h and obtain filter cake II, add the methyl alcohol agitator treating filter cake II of its quality 4 times, 1.2g Tea Polyphenols and 0.4g Vc sodium salt is added in solid after methanol wash, 1h is dried at 63 DEG C,
To product 27g, the mass percentage after testing containing lutein ester is 68%, wherein alltrans lutein: zeaxanthin (mol ratio)=91: 5.

Claims (1)

1. high-purity lutein ester composition and preparation technology, comprise the steps:
A. under 30 ~ 70 DEG C of conditions, marigold extractum is dissolved in mixed solvent A, adds adsorbent and stir 0.5 ~ 5 hour, filter, collect filtrate;
B. the filtrate of step a is cooled to 20 ~ 30 DEG C, keeps after 0.5 ~ 4 hour, then be cooled to 5 ~ 20 DEG C and keep 0.5 ~ 4 hour, filter to obtain filter cake I;
C., under 30 ~ 70 DEG C of conditions, dissolving filter cake I, in mixed solvent A, stirs and is cooled to 10 ~ 28 DEG C after 0.5 ~ 5 hour and keeps 0.5 ~ 5 hour, filter to obtain filter cake II;
D. use C1-3 alcohol washing leaching cake II, then add antioxidant, then the C1-3 alcohol that dry removing is residual, obtain the composition containing lutein ester;
Wherein said mixed solvent A is the mixed solvent of methyl acetate, ethyl acetate, n-propyl acetate or butyl acetate and C1-3 alcohol.
CN201310431363.6A 2013-09-22 2013-09-22 High-purity lutein ester composition and preparation process thereof Pending CN104432003A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113527166A (en) * 2021-08-26 2021-10-22 西安康诺化工有限公司 Preparation method of water-soluble lutein ester
US20220220059A1 (en) * 2021-01-14 2022-07-14 Kemin Industries, Inc. Process for crystallization of high purity lutein esters from marigold extracts

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220220059A1 (en) * 2021-01-14 2022-07-14 Kemin Industries, Inc. Process for crystallization of high purity lutein esters from marigold extracts
WO2022155338A1 (en) 2021-01-14 2022-07-21 Kemin Industries, Inc. Process for crystallization of high purity lutein esters from marigold extracts
CN113527166A (en) * 2021-08-26 2021-10-22 西安康诺化工有限公司 Preparation method of water-soluble lutein ester

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