CN1234713C - Process of extracting phosphatidylcholine from soybean phosphatide - Google Patents
Process of extracting phosphatidylcholine from soybean phosphatide Download PDFInfo
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- CN1234713C CN1234713C CN 02149601 CN02149601A CN1234713C CN 1234713 C CN1234713 C CN 1234713C CN 02149601 CN02149601 CN 02149601 CN 02149601 A CN02149601 A CN 02149601A CN 1234713 C CN1234713 C CN 1234713C
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Abstract
The present invention provides a method for extracting phosphatidyl choline from soybean phosphatide. Multi-stage counterflow extraction is carried out to soybean phospholipid by utilizing a double liquid phase mixed solvent comprising saturated alkane, acetonitrile and low-carbon alcohol, and then, vacuum exsolution is accomplished to a final extracting solution so as to obtain a product containing phosphatidyl choline for more than 80%. A yield is more than 80%. With the advantages of simple process, less investment for equipment and continuous and automatic operation, the method is suitable for large-scale industrialized production.
Description
Affiliated technical field
The present invention relates to the production method of phosphatidylcholine, especially relate to a kind of method of extracting phosphatidylcholine by soybean phospholipid.
Background technology
Phosphatidylcholine is one of of paramount importance composition in the phosphatide, is mainly used in industries such as protective foods, medicine, makeup.The method of extracting phosphatidylcholine at present mainly contains: column chromatography, salting-out process, supercritical extraction method, acetylation method, membrane separation process, solvent-extraction process etc.Column chromatography can prepare highly purified phosphatidylcholine product, but technology is amplified difficulty, and facility investment is bigger, is not suitable for large-scale industrial production.Salting-out process also can prepare highly purified phosphatidylcholine product, but its complex technical process, operational condition are harsh, the inorganic salt that use in the technology can cause environmental pollution.The supercritical extraction method equally also can prepare highly purified phosphatidylcholine product, yet supercritical extraction apparatus expensive, operational condition harshness are not suitable for large-scale promotion.Acetylation method utilizes the principle of chemical reaction to prepare highly purified phosphatidylcholine product, and higher to the purity requirement of raw material, chemical reaction influences the activity of phosphatide easily.The key of membrane separation process is a separatory membrane.But the present film of exploitation similar various phospholipid compositions of isolated molecule amount fully still, and transmitance is not high yet.Solvent-extraction process is the method for the industrial the most frequently used high-purity phosphatidylcholine of preparation, and concrete operations are convenient, be easy to industry amplifies, is easy to realize serialization and automatization.Its principle is to utilize the difference of each phospholipid fraction solubleness in specific solvent, and phosphatidylcholine and other components are separated.The common solvent of solvent-extraction process has: low-carbon alcohol, acetone, normal hexane, sherwood oil, ether, ethyl acetate etc.The topmost shortcoming of present disclosed solvent extraction process is: two indexs of the content of the phosphatidylcholine of products obtained therefrom and yield (yield=raw material phosphatidylcholine concentration * raw material weight/(product phosphatidylcholine concentration * product weight) * 100%) can not be taken into account, promptly when product purity was higher, product yield was lower; And when product yield was guaranteed, product purity was not high again.
Summary of the invention
The objective of the invention is in order to solve the problem that product yield and product purity are difficult to take into account simultaneously in the existing phosphatidylcholine production, by adopting solvent extraction process, and a kind of existing higher yields is provided, and the also higher method of product purity by soybean phospholipid extraction phosphatidylcholine.
The technical solution adopted in the present invention is as follows:
A kind of method by soybean phospholipid extraction phosphatidylcholine is characterized in that, adopts liquid-liquid extraction process, may further comprise the steps:
(1) soybean phospholipid is dissolved in alkane to obtain the stock liquid of 5-30% concentration, described alkane is C4-C10 saturated straight chain or branched paraffin, or their mixture; With acetonitrile and low-carbon alcohol is 1 by volume: 10-10: the 1 acetonitrile-low-carbon alcohol mixed solvent that mixes gained is as extraction agent, and described low-carbon alcohol is methyl alcohol, ethanol, propyl alcohol or their mixture;
(2) be 20-55 ℃ in temperature, the volume ratio of extraction agent and stock liquid is 1: 5-5: 1, and every grade of duration of contact is to carry out n stage countercurrent extracting operation under 0.2-3 hour the condition, wherein, 2≤n≤10;
(3) extraction liquid of n level is carried out the vacuum precipitation and promptly obtain the phosphatidylcholine product, its recovered solvent B returns the 1st grade and directly uses as extraction agent;
(4) the 1st grade raffinate is carried out the vacuum precipitation and promptly obtain other mixed phosphatide product, its recovered solvent A returns the n level directly as the solvent of preparation stock liquid.
Described soybean phospholipid can adopt common concentrating soya lecithin or powder soybean phospholipid.
Implement the method by soybean phospholipid extraction phosphatidylcholine of the present invention, can obtain phosphatidylcholine content and be higher than 80% phospholipid prod, the yield of phosphatidylcholine is not less than 80% simultaneously.In addition, owing to adopt liquid-liquid extraction process, extraction process is simple, and solvent load is few, is easy to realize industrialization and serialization production.
Description of drawings
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Fig. 1 is the present invention is extracted the method for phosphatidylcholine by soybean phospholipid a process flow sheet.
Embodiment
Embodiment 1
The phosphatide hexane solution that is mixed with 10% concentration with the powder soybean phospholipid that contains phosphatidyl choline 23% is as stock liquid, and the preparation acetonitrile: the extraction agent of ethanol=1: 3 (volume ratio).Adopt extraction agent: the charge ratio of stock liquid=1: 2 (volume ratio), at 30 ℃, under the condition of every grade of 60 minutes extraction time, carry out the extraction of 3 stage countercurrents by flow process shown in Figure 1.Products obtained therefrom detects through high performance liquid chromatography, and phosphatidylcholine content is 84.2%, and yield is 93%.
Embodiment 2
The phosphatide petroleum ether solution that is mixed with 20% concentration with the powder soybean phospholipid that contains phosphatidyl choline 23% is as stock liquid, and the preparation acetonitrile: the extraction agent of methyl alcohol=1: 6 (volume ratio).Adopt extraction agent: the charge ratio of stock liquid=1: 1 (volume ratio), at 40 ℃, under the condition of every grade of 30 minutes extraction time, carry out the extraction of 5 stage countercurrents by flow process shown in Figure 1.Products obtained therefrom detects through high performance liquid chromatography, and phosphatidylcholine content is 88.8%, and yield is 95%.
Embodiment 3
The phosphatide n-heptane solution that is mixed with 15% concentration with the powder soybean phospholipid that contains phosphatidyl choline 23% is as stock liquid, and the preparation acetonitrile: the extraction agent of n-propyl alcohol=5: 1 (volume ratio).Adopt extraction agent: the charge ratio of stock liquid=4: 1 (volume ratio), at 25 ℃, under the condition of every grade of 80 minutes extraction time, carry out the extraction of 6 stage countercurrents by flow process shown in Figure 1.Products obtained therefrom detects through high performance liquid chromatography, and phosphatidylcholine content is 93.5%, and yield is 85%.
Embodiment 4
The phosphatide isooctane solution that is mixed with 20% concentration with the powder soybean phospholipid that contains phosphatidyl choline 23% is as stock liquid, and the preparation acetonitrile: the extraction agent of Virahol=8: 1 (volume ratio).Adopt extraction agent: the charge ratio of stock liquid=4: 1 (volume ratio), at 25 ℃, under the condition of every grade of 100 minutes extraction time, carry out the extraction of 6 stage countercurrents by flow process shown in Figure 1.Products obtained therefrom detects through high performance liquid chromatography, and phosphatidylcholine content is 98.2%, and yield is 81%.
Embodiment 5
The phosphatide isopentane solution that is mixed with 25% concentration with the powder soybean phospholipid that contains phosphatidyl choline 23% is as stock liquid, and the preparation acetonitrile: methyl alcohol: the extraction agent of propyl alcohol=2: 1: 1 (volume ratio).Adopt extraction agent: the charge ratio of stock liquid=2: 1 (volume ratio), at 50 ℃, under the condition of every grade of 120 minutes extraction time, carry out the extraction of 10 stage countercurrents by flow process shown in Figure 1.Products obtained therefrom detects through high performance liquid chromatography, and phosphatidylcholine content is 95.1%, and yield is 92%.
Embodiment 6
Sherwood oil, acetonitrile, methyl alcohol mixed by 1: 2: 2 (volume ratio), obtain two liquid phases of equilibrated, it is standby to separate the back, and wherein rich sherwood oil is used for preparation raw material liquid mutually, and another is as extraction agent.Rich sherwood oil with powder soybean phospholipid that contains phosphatidyl choline 23% and above preparation is mixed with the phospholipid solution of 30% concentration mutually as stock liquid, adopt extraction agent: the charge ratio of stock liquid=1: 1 (volume ratio), at 55 ℃, under the condition of every grade of 150 minutes extraction time, carry out the extraction of 2 stage countercurrents by flow process shown in Figure 1.Products obtained therefrom detects through high performance liquid chromatography, and phosphatidylcholine content is 81.5%, and yield is 83%.
Embodiment 7
Octane, acetonitrile, ethanol mixed by 3: 5: 1 (volume ratio), obtain two liquid phases of equilibrated, it is standby to separate the back, and wherein rich octane is used for preparation raw material liquid mutually, and another is as extraction agent.Rich octane with powder soybean phospholipid that contains phosphatidyl choline 23% and above preparation is mixed with the phospholipid solution of 30% concentration mutually as stock liquid, adopt extraction agent: the charge ratio of stock liquid=2: 1 (volume ratio), at 45 ℃, under the condition of every grade of 50 minutes extraction time, carry out the extraction of 6 stage countercurrents by flow process shown in Figure 1.Products obtained therefrom detects through high performance liquid chromatography, and phosphatidylcholine content is 96.5%, and yield is 85%.
Claims (1)
1. the method by soybean phospholipid extraction phosphatidylcholine is characterized in that, adopts liquid-liquid extraction process, may further comprise the steps:
(1) soybean phospholipid is dissolved in alkane to obtain the stock liquid of 5-30% concentration, described alkane is C4-C10 saturated straight chain or branched paraffin, or their mixture; With acetonitrile and low-carbon alcohol is 1 by volume: 10-10: the 1 acetonitrile-low-carbon alcohol mixed solvent that mixes gained is as extraction agent, and described low-carbon alcohol is methyl alcohol, ethanol, propyl alcohol or their mixture;
(2) be 20-55 ℃ in temperature, the volume ratio of extraction agent and stock liquid is 1: 5-5: 1, and every grade of duration of contact is to carry out n stage countercurrent extracting operation under 0.2-3 hour the condition, wherein, 2≤n≤10;
(3) extraction liquid of n level is carried out the vacuum precipitation and promptly obtain the phosphatidylcholine product, its recovered solvent B returns the 1st grade and directly uses as extraction agent;
(4) the 1st grade raffinate is carried out the vacuum precipitation and promptly obtain other mixed phosphatide product, its recovered solvent A returns the n level directly as the solvent of preparation stock liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02149601 CN1234713C (en) | 2002-12-11 | 2002-12-11 | Process of extracting phosphatidylcholine from soybean phosphatide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02149601 CN1234713C (en) | 2002-12-11 | 2002-12-11 | Process of extracting phosphatidylcholine from soybean phosphatide |
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| CN1506368A CN1506368A (en) | 2004-06-23 |
| CN1234713C true CN1234713C (en) | 2006-01-04 |
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| CN 02149601 Expired - Fee Related CN1234713C (en) | 2002-12-11 | 2002-12-11 | Process of extracting phosphatidylcholine from soybean phosphatide |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104853614A (en) * | 2012-10-24 | 2015-08-19 | 卡吉尔公司 | Phospholipid-containing emulsifier composition |
| CN103288870B (en) * | 2013-05-08 | 2015-09-02 | 浙江大学 | A kind of preparation method of injection stage lecithin in high purity |
| CN103254227B (en) * | 2013-05-08 | 2016-06-08 | 浙江大学 | A kind of method adopting phenols extraction agent extracting and separating phosphatidylcholine |
| CN103265572B (en) * | 2013-05-08 | 2016-03-02 | 浙江大学 | A kind of method adopted containing carboxyl/polyhydroxyl solvents extraction separation purification phosphatidylcholine |
| CN105777804B (en) * | 2016-04-08 | 2018-08-28 | 合肥工业大学 | A kind of method of aqueous two-phase system purification egg yolk lecithin |
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