CN101955456A - Method for preparing high purity xanthophyll crystal - Google Patents
Method for preparing high purity xanthophyll crystal Download PDFInfo
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- CN101955456A CN101955456A CN2010105060725A CN201010506072A CN101955456A CN 101955456 A CN101955456 A CN 101955456A CN 2010105060725 A CN2010105060725 A CN 2010105060725A CN 201010506072 A CN201010506072 A CN 201010506072A CN 101955456 A CN101955456 A CN 101955456A
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Abstract
The invention provides a method for preparing high purity xanthophyll crystal. The method includes that: firstly ethanol and alkali are adopted to saponify marigold extract under the conditions of heating and stirring, reaction product is diluted by distilled water, and centrifugation, washing and vacuum drying are carried out, thus obtaining xanthophyll crystal crude product, wherein the content of xanthophylls is 70-80%, and the xanthophyll crystal is recrystallized by virtue of weak polar organic solvent and water, thus high purity xanthophyll product with the xanthophyll content of more than 90% is obtained. The process of the invention is simple, reaction condition is mild, and industrialized production is easy to realize. Xanthophyll product produced by the invention can be applied to the industries of feed, food, cosmetic and medicine.
Description
Technical field
The present invention relates to natural pigment crystalline process study, use technology of the present invention to prepare highly purified natural pigment from marigold extractum
Background technology
Xenthophylls (lutein) is a kind of carotenoid, and it extensively is present in the plants such as vegetables, flowers, fruit, belongs to " carotenoid " family material.Flower of Aztec Marigold is the main raw material that extracts xenthophylls, the xenthophylls that Flower of Aztec Marigold is extracted is non-harmful natural yellow pigment, have lovely luster, strong coloring force, safety non-toxic, antioxidant property excellence, advantage such as being rich in nutrition, can independently use, or be used with other materials, be widely used in many fields such as food, medicine, makeup, feed.
Studies show that, xenthophylls and zeaxanthin are unique carotenoid that is present in speckle regions in the human retina, xenthophylls causes that by oxidative damage macula retinae district the age danger of relevant maculopathy sex change (AMD) is relevant with reduction, xenthophylls can absorb blue light, reduce light to amphiblestroid damage, the visual deterioration that can be used for preventing senile macula retinae to degenerate causing and blind, delay the generation of eyes degenerative disease, also can effectively prevent the damage of ultraviolet ray human body skin; Xenthophylls has resists radical causes cell and organ damage in human body function, effectively diseases such as prevention of arterial sclerosis, coronary heart disease, tumour, cataract.
The extraction process of lutein extract is comparative maturity; and large-scale production already; but the preparation of high purity lutein crystal; also there is not the formal large-scale production of a family at present; major cause wherein is that production technique is ripe not enough,, long reaction time not high as product instability, yield, solvent cost height or the like.
The object of the present invention is to provide a kind of method that from the Flower of Aztec Marigold lutein extract, prepares high purity lutein crystal.
Operational path of the present invention comprises: under heating condition, alkali dissolution is behind alcohol, add lutein extract and stirring, make it to carry out saponification reaction, treat that saponification reaction is finished after, add hot distilled water, leave standstill after continuing to stir, the centrifugation lutein crystal is used the distilled water wash lutein crystal, vacuum-drying; Lutein crystal is dissolved in the organic solvent, adds water-alcohol solution and separate out until lutein crystal, with distilled water and washing with alcohol, vacuum-drying promptly gets the pure product of xenthophylls behind the centrifugal or suction filtration.
Therefore, the invention provides a kind of is raw material with the marigold extractum, prepares the method for high purity lutein crystal, it is characterized in that this method may further comprise the steps:
(1) with the marigold extractum is raw material, adopts ethanol and alkali, under heating condition, ten thousand medicinal extract are carried out saponification reaction;
(2) add distilled water, leave standstill;
(3) centrifugation lutein crystal;
(4) lutein crystal that obtains with the distilled water wash centrifugation.
(5) vacuum-drying (a 4) resulting lutein crystal;
(6) 5 resulting lutein crystals are dissolved in the weakly polar organic solvent, add entry alcohol mixed solution until precipitation occurring;
(7) suction filtration;
(8) use distilled water and washing with alcohol respectively;
(9) lutein crystal of 8 gained of vacuum-drying.
The method according to this invention, amount of alcohol added described in the wherein said step (1) are 1.5-3 times of lutein extract.
According to the process of claim 1 wherein that alkali described in the described step (1) is KOH, NaOH, Ca (OH)
2, carbonate etc., preferred KOH or NaOH, described concentration is 1.2-2.0mol/L.
According to the process of claim 1 wherein that the saponification reaction temperature is 55-60 ℃ described in the described step (1), the reaction times is 3-4 hour.
According to the process of claim 1 wherein that the middle distilled water that adds of described step (2) is hot distilled water, add-on is 4-10 a times of reaction mixture, and the control determining alcohol is 5-12%, continues stirring 10-30 minute behind the adding distilled water.
According to the process of claim 1 wherein in the described step (4) with distilled water wash 5-8 time, water become clarify till.
According to the process of claim 1 wherein that the middle weakly polar organic solvent of described step (6) is acetone, trichloromethane, ether ethyl ester, tetrahydrofuran (THF) etc., preferred tetrahydrofuran (THF) dissolves down at 60 ℃, and usage quantity is controlled at solid and just dissolves.
According to the process of claim 1 wherein that the middle water alcohol of described step (6) mixed solution is a 5-20% hexanol solution, add-on is till lutein crystal is separated out.
According to the process of claim 1 wherein that described step (5), (9) middle vacuum-drying are controlled at 38-45 ℃, time of drying is more than 24 hours.
The control of saponification temperature is crucial among the present invention, and temperature is lower than 55 ℃, and saponification is not thorough, and temperature is too high, and xenthophylls is easily degraded, and saponification time is controlled at 3-4 hour the best, and long xenthophylls degraded is serious.
Of the present invention to prepare the method production technique of purity xenthophylls from the Flower of Aztec Marigold lutein extract simple, and the reaction conditions gentleness easily realizes suitability for industrialized production, and the extraction yield height can reach more than 75%, and after testing, unified planning can reach more than 90%.
Embodiment
Embodiment 1:
Measure ethanol 1000ml, be heated to 60 ℃, add 120 gram KOH, stirring and dissolving takes by weighing 500 gram marigold extractum in alkaline solution, slowly stirs, and 55 ℃ of temperature controls reacted 3 hours.The hot distilled water 6L that adds 55 ℃, slowly stirred 15 minutes, left standstill 15 hours, centrifugal back is with distilled water wash 5 times, and recrystallization after the vacuum-drying is dissolved in crystal in 60 ℃ the tetrahydrofuran (THF), the alcoholic solution of adding 10% is to separating out crystallization, use distilled water and washing with alcohol behind the suction filtration, 42 ℃ of vacuum-dryings, the product body burden is 91%.
Embodiment 2:
Measure ethanol 100ml, be heated to 60 ℃, add 12 gram KOH, stirring and dissolving takes by weighing 50 gram marigold extractum in alkaline solution, slowly stirs, and 57 ℃ of temperature controls reacted 3.5 hours.The hot distilled water 800ml that adds 55 ℃, slowly stirred 10 minutes, left standstill 15 hours, centrifugal back is with distilled water wash 5 times, and recrystallization after the vacuum-drying is dissolved in crystal in 60 ℃ the tetrahydrofuran (THF), the alcoholic solution of adding 15% is to separating out crystallization, use distilled water and washing with alcohol behind the suction filtration, 42 ℃ of vacuum-dryings, crystalline content is 92%.
Claims (9)
1. the preparation method of a high purity lutein crystal is characterized in that:
(1) with the marigold extractum is raw material, adopts ethanol and alkali, under heating condition, marigold extractum is carried out saponification reaction;
(2) add distilled water, leave standstill;
(3) centrifugation lutein crystal;
(4) lutein crystal that obtains with the distilled water wash centrifugation.
(5) vacuum-drying (a 4) resulting lutein crystal;
(6) 5 resulting lutein crystals are dissolved in the weakly polar organic solvent, add entry alcohol mixed solution until precipitation occurring;
(7) suction filtration;
(8) use distilled water and washing with alcohol respectively;
(9) lutein crystal of 8 gained of vacuum-drying.
2. according to the process of claim 1 wherein 1.5-3 times that the middle amount of alcohol added of described step (1) is a lutein extract.
3. according to the process of claim 1 wherein that alkali is KOH or NaOH described in the described step (1), its concentration is 1.2-2.0mol/L.
4. according to the process of claim 1 wherein that the saponification reaction temperature is 55-60 ℃ described in the described step (1), the reaction times is 3-4 hour.
5. according to the process of claim 1 wherein that in the described step (2), adding distilled water is hot distilled water, add-on be reaction mixture 4-10 doubly, the control determining alcohol is 5-12%.
6. according to the process of claim 1 wherein in the described step (4) with distilled water wash 5-8 time, water become clarify till.
7. according to the process of claim 1 wherein that the middle weakly polar organic solvent of described step (6) is a tetrahydrofuran (THF), 60 ℃ of dissolvings down, usage quantity is controlled at solid and just dissolves.
8. according to the process of claim 1 wherein that the middle water alcohol of described step (6) mixed solution is the 5-15% ethanolic soln, add-on is till lutein crystal is separated out.
9. according to the process of claim 1 wherein that described step (5), (9) middle vacuum-drying temperature are controlled at 38-45 ℃, time of drying is more than 24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105060725A CN101955456A (en) | 2010-10-14 | 2010-10-14 | Method for preparing high purity xanthophyll crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105060725A CN101955456A (en) | 2010-10-14 | 2010-10-14 | Method for preparing high purity xanthophyll crystal |
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| CN101955456A true CN101955456A (en) | 2011-01-26 |
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| CN2010105060725A Pending CN101955456A (en) | 2010-10-14 | 2010-10-14 | Method for preparing high purity xanthophyll crystal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113234002A (en) * | 2021-04-24 | 2021-08-10 | 云南博浩生物科技集团股份有限公司 | Industrialized production method of lutein crystal |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5523494A (en) * | 1994-07-20 | 1996-06-04 | Industrial Organica, S.A. De C.V. | Process for the isomerization of lutein |
| CN1436774A (en) * | 2002-02-05 | 2003-08-20 | 海宁凤鸣叶绿素有限公司 | Lutein crystal preparing process from marigold flower |
| CN1603308A (en) * | 2004-06-03 | 2005-04-06 | 成都枫澜科技有限公司 | Method for preparing lutein crystal from marigold extractive |
| CN101429147A (en) * | 2008-11-18 | 2009-05-13 | 中国农业大学 | Method for producing high purity xanthophyll crystal with marigold oleoresin |
-
2010
- 2010-10-14 CN CN2010105060725A patent/CN101955456A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5523494A (en) * | 1994-07-20 | 1996-06-04 | Industrial Organica, S.A. De C.V. | Process for the isomerization of lutein |
| CN1436774A (en) * | 2002-02-05 | 2003-08-20 | 海宁凤鸣叶绿素有限公司 | Lutein crystal preparing process from marigold flower |
| CN1603308A (en) * | 2004-06-03 | 2005-04-06 | 成都枫澜科技有限公司 | Method for preparing lutein crystal from marigold extractive |
| CN101429147A (en) * | 2008-11-18 | 2009-05-13 | 中国农业大学 | Method for producing high purity xanthophyll crystal with marigold oleoresin |
Non-Patent Citations (1)
| Title |
|---|
| 张德君等: "叶黄素的提取及制备进展", 《化学工程师》, no. 7, 31 July 2005 (2005-07-31), pages 37 - 39 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113234002A (en) * | 2021-04-24 | 2021-08-10 | 云南博浩生物科技集团股份有限公司 | Industrialized production method of lutein crystal |
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Application publication date: 20110126 |