CN1035436C - Method for extracting high-purity lecithin with supercritical CO2 - Google Patents
Method for extracting high-purity lecithin with supercritical CO2 Download PDFInfo
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- CN1035436C CN1035436C CN94102372A CN94102372A CN1035436C CN 1035436 C CN1035436 C CN 1035436C CN 94102372 A CN94102372 A CN 94102372A CN 94102372 A CN94102372 A CN 94102372A CN 1035436 C CN1035436 C CN 1035436C
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- extraction
- yolk powder
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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
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention provides a method for extracting high-purity yolk phospholipid by supercritical CO2, which comprises the following steps that (a), yolk powder is used as raw materials, and CO2 is used as extraction agent, the extraction is carried out for 2 to 5 hours under the supercritical conditions of pressure of 25 to 35MPa and a temperature of 45 to 75DEGC, the neutral lipid is extracted, and yolk powder without lipid is obtained; (b), extraction solution is extracted from the yolk powder without neutral lipid by an extraction filtration method at normal temperature through using edible alcohol as extraction agent; (c) the highly-purity yolk phospholipid is prepared from the extraction solution by vacuum distillation or a spray drying method. The present invention has the advantages that the present invention reduces the extraction pressure and shortens the extraction time, the purity of the products is high, and the whole technological process can not cause unnecessary loss of phospholipid.
Description
The invention belongs to the edible phospholipid composition, be specifically related to a kind of method of producing high-purity lecithin.
Lecithin is the important additives in medicine, makeup and the food.Contain a large amount of lecithins very useful (about about 17Wt%) in the yolk to human body, also contain simultaneously a large amount of cholesterol (2-4Wt%) and glyceryl ester (＞40Wt%) etc. in character fat, character fat is to cause human body hyperlipidemia and hypertensive major cause in these.Extracting lecithin from yolk powder is the present comparatively general practice.Its method mainly is to adopt the organic solvent soaking extraction method to produce, and technological process is complicated, still contains higher cholesterol in the product.Even indicate 98.3% high-purity lecithin in Japan, also remaining 1.7% impurity, and this impurity nearly all is a cholesterol.In order to remove cholesterol, the spy opens clear 47-19062 and discloses a kind of method of extracting with acetone solvent, though the cholesterol level in the finished product has reduced, because the residual quantity of acetone is too big, human body still is harmful to.In order to solve residual noxious solvent problem, the spy opens clear 62-22556 and adopts supercritical CO
2Extractive method has extracted high-purity lecithin, and it is raw material with the yolk powder, carries out supercritical CO in two steps
2Extracting: the first step, with CO
2Be extractant, at pressure 400Kg/cm
2, temperature is that 40 ℃ of following extractings 5 hours are with character fat in removing; Second step is with CO
2With ethanol be extractant by the mixed solvent of the mixed of 10Wt%, at 400Kg/cm
2, 40 ℃ of following extractings 5 hours, products therefrom is removed ethanol through distillation, and to obtain purity be 98.7% lecithin.The advantage of this method is to have solved the residue problem of noxious solvent and obtained highly purified product, but it to exist a fatal shortcoming be industrial being difficult to realize that its major cause is: (1) extracting hypertonia reaches 400Kg/cm
2, industrial being difficult to realizes; (2) extracting overlong time, twice total 10 hours has a strong impact on output; (3) utilize this technological process, after a production cycle finishes, CO
2In contained a certain amount of ethanol, carry out next production cycle remove in during character fat, have the part lecithin certainly and extract, cause unnecessary phosphatide loss.
The objective of the invention is to overcome the defective of aforesaid method, the novel method of the extracting lecithin that a kind of processing condition realize easily, the operating process time is short, product purity is high is provided.
Supercritical CO of the present invention
2The method of extracting high-purity lecithin, carry out as follows:
(a) with the yolk powder be raw material, CO
2Be extractant,, under 45-75 ℃ the super critical condition, extracting 2-5 hour, the extracting of middle character fat gone out the yolk powder of character fat in obtaining removing at 25-35MPa;
(b) be extractant with the edible ethanol at normal temperatures with above-mentioned yolk powder, obtain extract with suction method;
(c) this extract is obtained highly purified lecithin through underpressure distillation or spray-drying process.
Method of the present invention roughly was divided into for two steps, and the first step is a supercritical CO
2Extracting, second step was underpressure distillation or a spraying drying behind the solvent extraction.Described the first step supercritical CO
2Extractive technical process as shown in drawings.1 is CO among the figure
2Basin, the 2nd, CO
2Pump, the 3rd, preheater, the 4th, under meter, the 5, the 6th, extractor, the 7, the 8th, separator.The present invention is raw materials used to be commercially available yolk powder, the CO that is adopted
2Purity＞99%.With the yolk powder extractor 5,6 of packing into, with circulating hot water heating preheater 3, extractor 5,6 and separator 7,8 to extraction temperature, the liquid CO in the basin
2Enter preheater 3 through pump 2 pressurization and be supercritical state, enter extractor 5 after the metering, reach extracting pressure after, middle character fat just is dissolved in supercritical CO
2In, and lecithin is insoluble, the outlet valve of slowly opening extractor 5 tops this moment keeps extracting pressure constant, makes the CO of character fat in being dissolved with
2Gas enters separator 7,8, makes it be step-down state step by step, and middle character fat is just separated from separator 7, and just separates from separator 8 automatically from the part moisture content that raw material comes.The CO that comes out from separator 8 tops
2Automatically returning to basin becomes aqueous recirculation to use.The continuous extracting of this closed cycle is time certain, and the middle character fat in the yolk powder just overwhelming majority is extracted.After extractor 5 extractings are intact, just can switch to extractor 6 and continue extracting, and extractor 5 is stand-by after raw material is changed in decompression.Middle character fat can be emitted from separator 7 bottoms, and moisture content is emitted from separator 8 bottoms, and whole process has just realized serialization, and character fat does not contain any organic solvent fully in the gained, and it is weak patient's a fabulous nutritive substance.
Second step was adopted the extractive method of nonpoisonous organic solvent, extracted highly purified lecithin in the yolk powder of character fat from remove.This step no longer takies supercritical CO
2Extraction plant, and adopt common solvent extraction process, its treatment capacity is increased greatly.With the yolk powder of character fat in removing at normal temperatures, with 3-5 purity doubly is that 95% edible ethanol carries out extracting, obtains extract with suction method, and the residue after the extracting is a vitellin(Vt), character fat content is the good additive of nutritive food seldom in the cholesterol etc.Extract just can obtain highly purified lecithin through underpressure distillation or spraying drying.
The present invention compared with prior art has following advantage: 1. reduced extracting pressure, made suitability for industrialized production become possibility; 2. make full use of the supercritical co extraction plant, shortened the extracting time, can improve output greatly; 3. the product purity height can not cause unnecessary phosphatide loss in whole technological process.
Embodiment 1
Commercially available yolk powder 200g goes into extractor, with the supercritical CO of purity＞99%
2Import, at 30MPa, 60 ℃ of following extractings 2.5 hours, in character fat 89.5g and remove in the yolk powder 110g of character fat.Is that 95% edible ethanol carries out solvent extraction with above-mentioned yolk powder with 3 times purity, and the gained extract gets lecithin 33.0g through underpressure distillation or spraying drying, the residual thing vitellin(Vt) 68.0g that heats up in a steamer.Do not contain any phosphatide in the character fat in the test by analysis, the purity of lecithin is 98.6%, and cholesterol level O.2%.
Embodiment 2
Commercially available yolk powder 200g is with the supercritical CO of purity＞99%
2At 35MPa, 50 ℃ of following extractings 2.5 hours, in character fat 89.6g, the yolk powder 110g of character fat in must removing.The gained yolk powder is 95% edible ethanol extracting with 4.5 times purity, the gained extract after underpressure distillation lecithin 33.5g, residue vitellin(Vt) 68.8g.Do not contain any phosphatide in the character fat in the test by analysis, the purity of lecithin is 98.7%, cholesterol level 0.2%.
The analytical procedure of product: the mensuration of lecithin is to record phosphorus content with the GB-5537-85 method earlier, calculates the content of lecithin again; Content of cholesterol is that the saponification of sample elder generation is separated, and goes out sterol with the reagent extracting again, by gas-chromatography, can record content of cholesterol.
Claims (2)
1. supercritical CO
2The method of extracting high-purity lecithin is characterized in that carrying out as follows:
(a) with the yolk powder be raw material, CO
2Be extractant,, under 45-75 ℃ the super critical condition, extracting 2-5 hour, the extracting of middle character fat gone out the yolk powder of character fat in obtaining removing at 25-35MPa;
(b) at normal temperatures with above-mentioned yolk powder, be extractant with the edible ethanol, obtain extract with suction method,
(c) this extract underpressure distillation or spraying drying are obtained highly purified lecithin.
2. the method for claim 1 is characterized in that the ratio of yolk powder and edible ethanol is 1: 3-5 in described (b) step solvent extraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94102372A CN1035436C (en) | 1994-03-07 | 1994-03-07 | Method for extracting high-purity lecithin with supercritical CO2 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94102372A CN1035436C (en) | 1994-03-07 | 1994-03-07 | Method for extracting high-purity lecithin with supercritical CO2 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1108258A CN1108258A (en) | 1995-09-13 |
| CN1035436C true CN1035436C (en) | 1997-07-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94102372A Expired - Fee Related CN1035436C (en) | 1994-03-07 | 1994-03-07 | Method for extracting high-purity lecithin with supercritical CO2 |
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| Country | Link |
|---|---|
| CN (1) | CN1035436C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012467A (en) * | 2011-09-20 | 2013-04-03 | 于殿宇 | Method for preparing high-purity acetylation soybean phospholipid under CO2 supercritical state |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1056375C (en) * | 1996-10-15 | 2000-09-13 | 中国人民解放军北京医学高等专科学校 | Refining process for high-purity yolk phospholipid |
| CN1048252C (en) * | 1997-09-08 | 2000-01-12 | 孙传经 | Method for extracting yolk lecithin from yolk with super-critical carbon dioxide |
| DE19854807A1 (en) * | 1998-11-27 | 2000-05-31 | Krupp Uhde Gmbh | Process for obtaining lecithin, in particular, from dry egg |
| CN1304398C (en) * | 2003-12-29 | 2007-03-14 | 黑龙江省大豆技术开发研究中心 | Supercritical CO2 extraction process for soya bean lecithin |
| CN103724369A (en) * | 2012-10-12 | 2014-04-16 | 广州白云山汉方现代药业有限公司 | Extraction method for yolk lecithin |
| CN104388188B (en) * | 2014-11-10 | 2017-04-12 | 大连工业大学 | Method for extracting triglyceride-type Antarctic krill oil and Antarctic krill phospholipid |
| CN106977541A (en) * | 2017-05-26 | 2017-07-25 | 贝因美婴童食品股份有限公司 | A kind of method for preparing long-chain polyunsaturated fatty acid phosphatide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6222556A (en) * | 1985-07-24 | 1987-01-30 | Daigo Eiyou Kagaku Kk | Production of high-purity egg yolk lecithin |
-
1994
- 1994-03-07 CN CN94102372A patent/CN1035436C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6222556A (en) * | 1985-07-24 | 1987-01-30 | Daigo Eiyou Kagaku Kk | Production of high-purity egg yolk lecithin |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012467A (en) * | 2011-09-20 | 2013-04-03 | 于殿宇 | Method for preparing high-purity acetylation soybean phospholipid under CO2 supercritical state |
| CN103012467B (en) * | 2011-09-20 | 2015-12-16 | 于殿宇 | A kind of at CO 2the method of highly acetylated soybean phospholipid is prepared under supercritical state |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1108258A (en) | 1995-09-13 |
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