CN101139312A - Method for preparing free lutein having high saponification ratio - Google Patents
Method for preparing free lutein having high saponification ratio Download PDFInfo
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- CN101139312A CN101139312A CNA2007100721749A CN200710072174A CN101139312A CN 101139312 A CN101139312 A CN 101139312A CN A2007100721749 A CNA2007100721749 A CN A2007100721749A CN 200710072174 A CN200710072174 A CN 200710072174A CN 101139312 A CN101139312 A CN 101139312A
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- saponification
- lutein
- certain
- xenthophylls
- organic solvent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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Abstract
The present invention provides a preparation method of the free lutein with the high rate of saponification. At first, the lutein ointment is mixed with the organic solvent according to a certain proportion; after preheating, a certain amount of alkaline solution is added; the negative-pressure return and saponification reaction is done with the nitrogen protection at a certain temperature and under the negative-pressure conditions; after a certain time of the saponification reaction, the saponification reaction is stopped; the pH value of the solution is adjusted to be neutral after the saponification; the static delamination is done to get the saponified free lutein; the saponification rate in one production process can reach 90 to 95 percent; the collection rate of the lutein can reach above 90 percent; the technical index and the product performance both achieve the leading level at home and the advanced level in the similar category abroad. In the present invention, with the use of the nitrogen protection and the negative-pressure return and saponification reaction, the invention is characterized in the simple process, the small amount of the used solvent and the high saponification rate of the product, wherein the most prominent feature is that the method greatly shortens the saponification time; the effective ingredient free lutein can be fully maintained; the method is easy for the industrial production.
Description
Affiliated technical field:
The present invention relates to a kind of lutein ester saponification production technique.Particularly adopted negative pressure backflow saponification reaction improved greatly the saponification degree of lutein ester, greatly shortened saponification send out seasonable between, adopted the loss of nitrogen protection product xenthophylls few simultaneously, the yield height is easy to preparation technology's industrialization of Flower of Aztec Marigold free lutein.
Background technology:
Xenthophylls belongs to the tetraterpenes compound of carotenoid class, and Flower of Aztec Marigold is the main raw material that extracts carotenoid (xenthophylls).The xenthophylls that Flower of Aztec Marigold is extracted is non-harmful natural yellow pigment, and coloring effect is good, can independently use or be used with other pigment.
The higher smart powder of Leaf of Aztec Marigold flavine of purity is orange-yellow powder, and weak hay smell is arranged, and xenthophylls has two kinds of existence forms, free state and lutein ester in the plant materials; Free lutein can directly be absorbed by human body and bird, and the xenthophylls that exists with the lutein ester form is difficult for being absorbed by human body and animal, just can be absorbed after having only lutein ester to be hydrolyzed into free lutein.
At present, the research and the production technique of xenthophylls are varied both at home and abroad.Difference according to the xenthophylls production process is divided into two big classes: 1) extraction of xenthophylls and saponification are carried out simultaneously; 2) saponification of the extraction of xenthophylls and xenthophylls separates and carries out.Difference according to the saponification solvent system of xenthophylls is divided into three major types: 1) buck system saponification process; 2) the NaOH aqueous solution-propyl carbinol system saponification process; 3) KOH methanol solution system saponification process.All there are pros and cons separately in above-mentioned xenthophylls saponification process in actual production,, problem such as solvent loss big, saponification temperature too high, saponification degree low and yield not high long as saponification time, xenthophylls products production cost is too high to cause the xenthophylls industry development slow, can't satisfy the growing market requirement.
It is simple that the present invention has technical process; solvent load is few; particularly adopted negative pressure backflow saponification reaction improved greatly the saponification degree of lutein ester, greatly shortened saponification send out seasonable between; adopted the loss of nitrogen protection product xenthophylls few simultaneously; the yield height is easy to the advantage of preparation technology's industrialization of Flower of Aztec Marigold free lutein.
The mechanism of negative pressure backflow saponification reaction is as follows:
By the negative pressure of vacuum saponification process, (xenthophylls also is heat-sensitive substance for needed temperature and saponification time when having reduced the xenthophylls saponification, too high or the long-time high temperature action of temperature generates isomer, lose original activity), also simplified simultaneously production technique, avoided repeatedly repeating to extract the saponification process, reduced the loss of xenthophylls, made xenthophylls saponification degree and yield improve greatly.
Summary of the invention:
The object of the invention is to provide that a kind of technical process is simple, solvent load is few, saponification time is short, the Flower of Aztec Marigold free lutein preparation technology method of high lutein saponification degree and high yield.
In order to achieve the above object; the technical solution used in the present invention is: lutein factice is mixed with organic solvent by a certain percentage; through after the preheating; add certain amount of alkaline solution again; under nitrogen protection, certain temperature and condition of negative pressure, carry out negative pressure backflow saponification reaction; stop saponification reaction when reaching certain saponification reaction after time; the pH value of solution value is neutral after the adjusting saponification; carry out static layering and obtain the saponification free lutein; the xenthophylls saponification degree of a production process can reach 90～95%, and the xenthophylls yield reaches more than 90%.
Described lutein factice is the lutein factice (medicinal extract) that obtains after the marigold flower particle concentrates through extraction with organic solvent.
Described certain proportion is that lutein factice and organic solvent volume ratio are 1: 0.5～8
Described organic solvent is hydrocarbon organic solvents such as sherwood oil, normal hexane.
Described certain amount of alkaline solution can be sodium hydroxide-ethanol system, potassium hydroxide-methanol system, sodium hydroxide-basic solution systems such as butanols system.
Described processing method, wherein said certain temperature are 20～90 ℃.
Advantage of the present invention:
1, owing in whole preparation xenthophylls process, adopted the nitrogen protection method, effectively completely cut off contacting of oxygen in xenthophylls and the air, reduced the degraded of xenthophylls and the appearance of isomer, make effective xenthophylls amount increase.
2, by the negative pressure of vacuum saponification process, (xenthophylls also is heat-sensitive substance for needed temperature and saponification time when having reduced the xenthophylls saponification, too high or the long-time high temperature action of temperature generates isomer, lose original activity), also simplified simultaneously production technique, avoided repeatedly repeating to extract the saponification process, reduced the loss of xenthophylls, made xenthophylls saponification degree and yield improve greatly.
3, it is few to have a solvent load, all recyclable utilization of all ingredients, and cost is low.
Specific embodiments:
Below embodiment of the present invention are further described:
With lutein factice (lutein factice: organic solvent=1: 0.5～8) mix in proportion with organic solvent; through after the preheating; add certain amount of alkaline solution again; under nitrogen protection, certain temperature and condition of negative pressure, carry out negative pressure backflow saponification reaction; stop saponification reaction when reaching certain saponification reaction after time; the pH value of solution value is neutral after the adjusting saponification; carry out static layering and obtain the saponification free lutein; the xenthophylls saponification degree of a production process can reach 90～95%, and the xenthophylls yield reaches more than 90%.
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1
Get lutein factice 50g; add the 70mL sherwood oil; behind the preheating thorough mixing; adding concentration is 20% sodium hydroxide-ethanolic soln 10mL; in nitrogen protection; temperature is 60 ℃, and negative pressure is a negative pressure backflow saponification reaction under the 0.04MPa condition, reaches 4 hours when the saponification reaction time; stop saponification reaction; adding acetate and adjust the pH value of solution after the saponification, be neutrality up to the pH value of solution value, and the sodium chloride aqueous solution of 3～4 times 10% of gradation adding washs again; static layering; obtain upper strata saponification free lutein, the xenthophylls saponification degree of one time production process can reach 94.2%, and the xenthophylls yield reaches 95%.
Embodiment 2
Get lutein factice 30g; add the 60mL normal hexane; behind the preheating thorough mixing; adding concentration is 20% potassium hydroxide-methanol solution 5mL; in nitrogen protection; temperature is 50 ℃, and negative pressure is a negative pressure backflow saponification reaction under the 0.03MPa condition, reaches 4 hours when the saponification reaction time; stop saponification reaction; adding acetate and adjust the pH value of solution after the saponification, be neutrality up to the pH value of solution value, and the sodium chloride aqueous solution of 3～4 times 10% of gradation adding washs again; static layering; obtain upper strata saponification free lutein, the xenthophylls saponification degree of one time production process can reach 95.4%, and the xenthophylls yield reaches 95.6%.
Claims (6)
1. the preparation method of the free lutein of a high saponification ratio; it is characterized in that: earlier lutein factice is mixed with organic solvent by a certain percentage; through after the preheating; add certain amount of alkaline solution again; under nitrogen protection, certain temperature and condition of negative pressure, carry out negative pressure backflow saponification reaction; stop saponification reaction when reaching certain saponification reaction after time; the pH value of solution value is neutral after the adjusting saponification; carry out static layering and obtain the saponification free lutein; the xenthophylls saponification degree of a production process can reach 90～95%, and the xenthophylls yield reaches more than 90%.
2. according to the described processing method of claim 1, wherein said lutein factice is the lutein factice (medicinal extract) that obtains after the marigold flower particle concentrates through extraction with organic solvent.
3. according to the described processing method of claim 1, wherein said certain proportion is that lutein factice and organic solvent volume ratio are 1: 0.5～8.
4. according to the described processing method of claim 1, wherein said organic solvent is hydrocarbon organic solvents such as sherwood oil, normal hexane.
5. according to the described processing method of claim 1, wherein said certain amount of alkaline solution can be sodium hydroxide-ethanol system, potassium hydroxide-methanol system, sodium hydroxide-basic solution systems such as butanols system.
6. according to the described processing method of claim 1, wherein said certain temperature is 20～90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100721749A CN101139312A (en) | 2007-05-08 | 2007-05-08 | Method for preparing free lutein having high saponification ratio |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100721749A CN101139312A (en) | 2007-05-08 | 2007-05-08 | Method for preparing free lutein having high saponification ratio |
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| CN101139312A true CN101139312A (en) | 2008-03-12 |
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| CNA2007100721749A Pending CN101139312A (en) | 2007-05-08 | 2007-05-08 | Method for preparing free lutein having high saponification ratio |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979377A (en) * | 2010-09-20 | 2011-02-23 | 广州智特奇生物科技有限公司 | Method for saponifying lutein grease |
| CN103772253A (en) * | 2012-10-19 | 2014-05-07 | 哈尔滨理工大学 | Preparation method of xanthophyll |
| CN106316909A (en) * | 2016-08-19 | 2017-01-11 | 晨光生物科技集团股份有限公司 | Continuous lutein extract saponifying process |
| WO2017005087A1 (en) * | 2015-07-09 | 2017-01-12 | 浙江新维普添加剂有限公司 | Lutein feed additive preparation method |
-
2007
- 2007-05-08 CN CNA2007100721749A patent/CN101139312A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979377A (en) * | 2010-09-20 | 2011-02-23 | 广州智特奇生物科技有限公司 | Method for saponifying lutein grease |
| CN101979377B (en) * | 2010-09-20 | 2013-12-25 | 广州智特奇生物科技有限公司 | Method for saponifying lutein grease |
| CN103772253A (en) * | 2012-10-19 | 2014-05-07 | 哈尔滨理工大学 | Preparation method of xanthophyll |
| CN103772253B (en) * | 2012-10-19 | 2015-12-16 | 哈尔滨理工大学 | A kind of preparation method of xenthophylls |
| WO2017005087A1 (en) * | 2015-07-09 | 2017-01-12 | 浙江新维普添加剂有限公司 | Lutein feed additive preparation method |
| CN106316909A (en) * | 2016-08-19 | 2017-01-11 | 晨光生物科技集团股份有限公司 | Continuous lutein extract saponifying process |
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