CN106632457B - A kind of method by the purifying high-purity egg yolk lecithin that is demulsified - Google Patents
A kind of method by the purifying high-purity egg yolk lecithin that is demulsified Download PDFInfo
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- CN106632457B CN106632457B CN201611015016.5A CN201611015016A CN106632457B CN 106632457 B CN106632457 B CN 106632457B CN 201611015016 A CN201611015016 A CN 201611015016A CN 106632457 B CN106632457 B CN 106632457B
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- JQWAHKMIYCERGA-UHFFFAOYSA-N (2-nonanoyloxy-3-octadeca-9,12-dienoyloxypropoxy)-[2-(trimethylazaniumyl)ethyl]phosphinate Chemical compound CCCCCCCCC(=O)OC(COP([O-])(=O)CC[N+](C)(C)C)COC(=O)CCCCCCCC=CCC=CCCCCC JQWAHKMIYCERGA-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 27
- 235000010445 lecithin Nutrition 0.000 claims abstract description 101
- 239000000787 lecithin Substances 0.000 claims abstract description 101
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims abstract description 90
- 229940067606 lecithin Drugs 0.000 claims abstract description 89
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 claims abstract description 50
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000012043 crude product Substances 0.000 claims abstract description 41
- 239000003925 fat Substances 0.000 claims abstract description 34
- 230000007935 neutral effect Effects 0.000 claims abstract description 33
- 235000012000 cholesterol Nutrition 0.000 claims abstract description 25
- 150000003626 triacylglycerols Chemical class 0.000 claims abstract description 24
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 15
- 239000000839 emulsion Substances 0.000 claims abstract description 9
- 235000013601 eggs Nutrition 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- 210000002969 egg yolk Anatomy 0.000 claims description 28
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 19
- 238000000605 extraction Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- 102000002322 Egg Proteins Human genes 0.000 claims description 9
- 108010000912 Egg Proteins Proteins 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- 239000000469 ethanolic extract Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 230000001954 sterilising effect Effects 0.000 claims description 6
- 238000004659 sterilization and disinfection Methods 0.000 claims description 6
- 229940037003 alum Drugs 0.000 claims description 5
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 5
- 206010054949 Metaplasia Diseases 0.000 abstract description 4
- 230000015689 metaplastic ossification Effects 0.000 abstract description 4
- 238000000703 high-speed centrifugation Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000012567 medical material Substances 0.000 abstract description 3
- 238000002481 ethanol extraction Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000000284 extract Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 230000006837 decompression Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000001164 aluminium sulphate Substances 0.000 description 2
- 235000011128 aluminium sulphate Nutrition 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 210000004681 ovum Anatomy 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 150000003904 phospholipids Chemical class 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- -1 Acyl monoethanolamine Chemical compound 0.000 description 1
- 241000272525 Anas platyrhynchos Species 0.000 description 1
- 241000272814 Anser sp. Species 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 241000286209 Phasianidae Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 210000004958 brain cell Anatomy 0.000 description 1
- 210000005013 brain tissue Anatomy 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013345 egg yolk Nutrition 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 210000004126 nerve fiber Anatomy 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 230000001537 neural effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/10—Phosphatides, e.g. lecithin
- C07F9/103—Extraction or purification by physical or chemical treatment of natural phosphatides; Preparation of compositions containing phosphatides of unknown structure
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Fats And Perfumes (AREA)
- Meat, Egg Or Seafood Products (AREA)
Abstract
The invention belongs to medical material processing technique field, specifically, is related to a kind of method by the purifying high-purity egg yolk lecithin that is demulsified.This method is further to be refined the lecithin crude product obtained by ethanol extraction, supercritical carbon dioxide extracting, its significant progress is to employ sulfate, the emulsion system for forming the neutral fats such as lecithin and minimal amount of triglycerides, the cholesterol in lecithin crude product destroys, so that the lecithin in lecithin crude product is separated with neutral fats, further cooled by two level, by neutral fats such as minimal amount of triglycerides, cholesterol except taking off under the conditions of high speed centrifugation, so as to refine out high-purity egg yolk lecithin.The purity of product brings up to more than 98%, realize high-purity egg yolk lecithin clean, pollution-free metaplasia production, fully meet lecithin product and used as medicinal raw material.
Description
Technical field
The invention belongs to medical material processing technique field, specifically, is related to one kind by the purifying high-purity egg that is demulsified
The method of yellow lecithin.
Background technology
Lecithin is the basic substance of life, is present among each cell, is the important component for forming nerve fiber, belongs to
In neural high-grade nutrient element.Therefore supplement lecithin can activate brain cell, dispelling fatigue, enhancing memory, the improvement state of mind, from
And keep the health of brain tissue and nervous system.In view of the function that lecithin is special, is increasingly turned to medicine by health products at present.
, can be with dissolving cholesterol, triglycerides etc. because its emulsification to fat strength, therefore to mitigating vascular wall lipoids, press down
Braking pulse atherosclerosis have obvious action.
In order to which more suitable for medicinal, the egg yolk lecithin with more preferable bioactivity and human body utilization rate grinds as emphasis
Study carefully object.Although the method for extraction egg yolk lecithin is more at present, purity is relatively low, it is difficult to the requirement met.Pass
The method of the extraction egg yolk lecithin of system typically uses organic solvent method, and the egg yolk lecithin of acquisition is enriched cholesterol etc., therefore
Purity is low, and it is usually acetone to use solvent, introduces poisonous and harmful solvent, so not only results in organic solvent in the product
Residual, and cause environmental pollution.
Chinese invention patent CN101029057A discloses a kind of preparation method of egg yolk lecithin, and this method is with fowl
Egg is raw material, isolates yolk and stirs into egg yolk liquid, extracted with edible alcohol, isolates extract solution, and extract solution is concentrated, is dehydrated
Lecithin first product is obtained, lecithin first product is subjected to supercritical CO 2 extraction again, removes neutral fat, removing neutral fat is made
Lecithin, but the egg yolk lecithin purity that this method obtains still can not meet pharmaceutical requirement.
Chinese invention patent CN1733777A discloses a kind of preparation method of high-purity egg yolk lecithin, including 1) new
Fresh yolk first uses acetone degreasing, vacuum filtration, filter cake alcoholic extraction, merging filtrate, and vacuum concentration obtains raw phospholipid；2) pass through
The aluminum oxide of passivation fills post with methanol wet, is first rinsed with methanol；3) chromatographic column is added after raw phospholipid is dissolved with methanol, and is opened
Begin to collect efflux；4) rinsed after lecithin starts to penetrate with pure methanol, collect efflux.Caused using acetone degreasing
Poisonous substance remains, and has pollution to environment.
Chinese invention patent CN102924506 A disclose a kind of preparation method of high purity lecithin, are moved using simulation
Dynamic bed continuous chromatography isolation technics ensures that lecithin efficiently separates with contained other compositions in starting lipid, obtains high-purity
Lecithin product.This method complex process, although purity is high, efficiency is low, it is difficult to meets the requirement of scale extraction.
Therefore, to extract high-purity egg yolk lecithin significant to developing medicinal lecithin for pollution-free, efficient, scale, and
Prior art can't fully meet the demand.
The content of the invention
Complicated for current egg yolk lecithin process for refining, the defects of easily causing secondary pollution, the present invention proposes one
The method that kind passes through the purifying high-purity egg yolk lecithin that is demulsified.The characteristics of it is protruded is solid to triglycerides, courage for lecithin
The neutral fats such as alcohol have an extremely strong emulsifying capacity, and the neutral grease such as lecithin and triglycerides, cholesterol is difficult in lecithin crude product
With the characteristic of separation, it is demulsified by using sulfate, by the neutral fats such as minimal amount of triglycerides, cholesterol in lecithin crude product
Isolate, it is achieved thereby that cleaning, pollution-free metaplasia produces high-purity egg yolk lecithin.Obtained purity of lecithin is complete more than 98%
Full up sufficient lecithin product uses as medicinal raw material.
To achieve these goals, the present invention uses following technical scheme：
A kind of method by the purifying high-purity egg yolk lecithin that is demulsified, it is characterised in that：Specific extracting method is as follows：
（1）The egg washing that low temperature is stored, ultraviolet sterilization is carried out, yolk is isolated under whole vacuum condition, by egg
Yellow and volumetric concentration is 90-95% ethanol with volume ratio 1:5-10 add high speed dispersor, high speed dispersor temperature it is constant
It is 15-20 DEG C, scattered at a high speed with 5000-10000rpm rotating speed, the lecithin in yolk is kept completely separate with egg yolk protein, point
Time 30-45min is dissipated, then stands 15min, ethanol extracts the mixed liquor comprising egg oil and lecithin from yolk；
（2）By step（1）Vacuum-concentrcted is to paste under the conditions of 30-35 DEG C for obtained mixed liquor, further 45
It is dried in vacuo, crushes under the conditions of DEG C, obtains powdered lecithins mixture；
（3）By step（2）Obtained powdered lecithins mixture adds extraction kettle, is passed through liquid carbon dioxide and carries out super face
Boundary extracts egg oil, and carbon dioxide is sent into separator with egg oil fluid-mixing, and further pressure release causes carbon dioxide and yolk
Oil is rapidly separated, and reclaims egg oil；Collected in extraction kettle and obtain lecithin crude product；
（4）In step（3）The ethanol that volumetric concentration is 80-85% is added in obtained lecithin crude product, control ethanol adds
Amount, viscosity 10-15cP solution is mixed to get with lecithin crude product, then adds sulfate, makes the lecithin in lecithin crude product
The emulsion system that the neutral fats such as fat and minimal amount of triglycerides, cholesterol is formed destroys；
（5）Temperature is further reduced, carries out two-stage centrifugal processing：
The first order：Under the conditions of -30 DEG C with 2000-3000rpm centrifugal speed under centrifuge, by minimal amount of with cholesterol
Based on neutral fats except de-, obtain clear liquid；
The second level：The clear liquid that the first order is obtained is centrifuged under the conditions of -50 DEG C with 4000-5000rpm centrifugal speed, will
The minimal amount of neutral fats based on triglycerides courage is except de-；
（6）By step（5）By the solution that two-stage centrifugal obtains by being dried under reduced pressure, washing, ethyl acetate is washed, decompression is done
It is dry to obtain refined high-purity egg yolk lecithin.
Preferably, step（4）Described sulfate is at least one of aluminum sulfate, alum.
Preferably, step（4）Described sulfate addition is the 3-5% of lecithin crude product solution quality.
Preferably, step（4）Described sulfate is the fine powder that particle diameter is less than 5 microns.
Further preferably, step（4）Described sulfate is nanometer grade powder.
Preferably, step（5）Described first order centrifugal speed is 2500rpm.
Preferably, step（5）Described second level centrifugal speed is 4500rpm.
Lecithin is due to having extremely strong emulsifying capacity, therefore the ovum in lecithin crude product to triglycerides, cholesterol etc.
Phosphatide is emulsified homogeneously to exist with neutral greases such as triglycerides, cholesterol, although big except having taken off by supercritical carbon dioxide
Part egg oil, but the quality that the neutral greases such as a small amount of triglycerides, cholesterol have impact on lecithin is remained, cause lecithin
Purity is low, can not be used as medical material.
The characteristics of present invention is prominent is to enter the lecithin crude product obtained by ethanol extraction, supercritical carbon dioxide extracting
One step is refined, and its significant progress is to employ sulfate, make lecithin in lecithin crude product with it is minimal amount of sweet
The emulsion system that the neutral fats such as oily three esters, cholesterol are formed destroys, so that the lecithin in lecithin crude product goes out with neutral fats
Now it is separated, is further cooled by two level, by neutral fats such as minimal amount of triglycerides, cholesterol under the conditions of high speed centrifugation
Except taking off, so as to refine out high-purity egg yolk lecithin.
One typical operational instances, makes the purity of product bring up to more than 98%, and it is clear to realize high-purity egg yolk lecithin
Clean, the production of pollution-free metaplasia, fully meet lecithin product and are used as medicinal raw material.Significantly more advantage is to refine
Cleaned in journey using ethyl acetate, effectively prevent lecithin from being influenceed by extraneous oxygen, water environment, preferably ensure that lecithin
Activity, extend its pot-life.
A kind of method by the purifying high-purity egg yolk lecithin that is demulsified of the invention, compared with prior art its spy protruded
Point and excellent effect are shown：
1st, sulfate is employed, makes the neutrality such as lecithin and minimal amount of triglycerides, cholesterol in lecithin crude product
The emulsion system that fat is formed destroys, so that the lecithin in lecithin crude product is separated with neutral fats, further passes through
Two level cools, and removes the neutral fats such as minimal amount of triglycerides, cholesterol under the conditions of high speed centrifugation and takes off, high-purity so as to refine out
Spend egg yolk lecithin.
2nd, cleaned in subtractive process using ethyl acetate, effectively prevent lecithin from being influenceed by extraneous oxygen, water environment, preferably
The activity that ensure that lecithin, extend its pot-life.
3rd, preparation method provided by the invention, realize high-purity egg yolk lecithin clean, pollution-free metaplasia production, it is completely full
Sufficient lecithin product uses as medicinal raw material.
Embodiment
Below by way of specific embodiment, the present invention will be further explained, but this should not be interpreted as into the scope of the present invention
It is only limitted to following embodiment.In the case where not departing from above method thought of the present invention, according to ordinary skill knowledge
The various replacements or change made with customary means, should be included in the scope of the present invention.
Embodiment 1
（1）The egg of low temperature storage is cleaned, ultraviolet sterilization is carried out, yolk is isolated under whole vacuum condition, by egg
The ethanol that yellow and volumetric concentration is 95% is with volume ratio 1:5 add high speed dispersor, and high speed dispersor temperature is constant at 15-20 DEG C,
It is scattered at a high speed with 5000rpm rotating speed, the lecithin in yolk is kept completely separate with egg yolk protein, jitter time 30min, so
After stand 15min, ethanol extracts the mixed liquor comprising egg oil and lecithin from yolk；
（2）By step（1）Vacuum-concentrcted is to paste under the conditions of 30-35 DEG C for obtained mixed liquor, further 45
It is dried in vacuo, crushes under the conditions of DEG C, obtains powdered lecithins mixture；
（3）By step（2）Obtained powdered lecithins mixture adds extraction kettle, is passed through liquid carbon dioxide and carries out super face
Boundary extracts egg oil, and carbon dioxide is sent into separator with egg oil fluid-mixing, and further pressure release causes carbon dioxide and yolk
Oil is rapidly separated, and reclaims egg oil；Collected in extraction kettle and obtain lecithin crude product；
（4）In step（3）The ethanol that volumetric concentration is 80% is added in obtained lecithin crude product, controls amount of alcohol added,
Viscosity 10cP solution is mixed to get with lecithin crude product, then adds the Aluminium Sulphate usp (powder) that particle diameter is less than 5 μm, is made by stirring
The emulsion system that the neutral fats such as lecithin and minimal amount of triglycerides, cholesterol in lecithin crude product are formed destroys；Sulfuric acid
Aluminium addition is the 3% of lecithin crude product solution quality.
（5）Temperature is further reduced, carries out two-stage centrifugal processing：
The first order：Under the conditions of -30 DEG C with 2500rpm centrifugal speed under centrifuge, by minimal amount of based on cholesterol
Neutral fats except de-, obtain clear liquid；
The second level：The clear liquid that the first order is obtained is centrifuged under the conditions of -50 DEG C with 4500rpm centrifugal speed, will be few
The neutral fats based on triglycerides courage of amount is except de-；
（6）By step（5）By the solution that two-stage centrifugal obtains by being dried under reduced pressure, washing, ethyl acetate is washed, decompression is done
It is dry to obtain refined high-purity egg yolk lecithin.
By being examined to the fine egg yolk lecithin of collection, product purity has reached 98.5%.
Embodiment 2
（1）The goose egg of low temperature storage is cleaned, ultraviolet sterilization is carried out, yolk is isolated under whole vacuum condition, by egg
The ethanol that yellow and volumetric concentration is 95% is with volume ratio 1:8 add high speed dispersor, and high speed dispersor temperature is constant at 15-20 DEG C,
It is scattered at a high speed with 10000rpm rotating speed, the lecithin in yolk is kept completely separate with egg yolk protein, jitter time 45min,
Then 15min is stood, ethanol extracts the mixed liquor comprising egg oil and lecithin from yolk；
（2）By step（1）Vacuum-concentrcted is to paste under the conditions of 30-35 DEG C for obtained mixed liquor, further 45
It is dried in vacuo, crushes under the conditions of DEG C, obtains powdered lecithins mixture；
（3）By step（2）Obtained powdered lecithins mixture adds extraction kettle, is passed through liquid carbon dioxide and carries out super face
Boundary extracts egg oil, and carbon dioxide is sent into separator with egg oil fluid-mixing, and further pressure release causes carbon dioxide and yolk
Oil is rapidly separated, and reclaims egg oil；Collected in extraction kettle and obtain lecithin crude product；
（4）In step（3）The ethanol that volumetric concentration is 85% is added in obtained lecithin crude product, controls amount of alcohol added,
Viscosity 15cP solution is mixed to get with lecithin crude product, alum nano powder is then added, makes the ovum in lecithin crude product
The emulsion system that the neutral fats such as phosphatide and minimal amount of triglycerides, cholesterol is formed destroys；Alum addition is lecithin
The 5% of fat crude product solution quality.
（5）Temperature is further reduced, carries out two-stage centrifugal processing：
The first order：Under the conditions of -30 DEG C with 3000rpm centrifugal speed under centrifuge, by minimal amount of based on cholesterol
Neutral fats except de-, obtain clear liquid；
The second level：The clear liquid that the first order is obtained is centrifuged under the conditions of -50 DEG C with 5000rpm centrifugal speed, will be few
The neutral fats based on triglycerides courage of amount is except de-；
（6）By step（5）By the solution that two-stage centrifugal obtains by being dried under reduced pressure, washing, ethyl acetate is washed, decompression is done
It is dry to obtain refined high-purity egg yolk lecithin.
By carrying out conventional detection to the fine egg yolk lecithin of collection, its composition is：Containing phosphatidyl choline 98.0%, phosphorus
Acyl monoethanolamine 0.5%, Lysophosphatidylcholone 0.5%.
Embodiment 3
（1）The quail egg of low temperature storage is cleaned, ultraviolet sterilization is carried out, yolk is isolated under whole vacuum condition, will
The ethanol that yolk and volumetric concentration are 90% is with volume ratio 1:10 add high speed dispersor, and high speed dispersor temperature is constant in 15-20
DEG C, it is scattered at a high speed with 8000rpm rotating speed, the lecithin in yolk is kept completely separate with egg yolk protein, jitter time
30min, then stands 15min, and ethanol extracts the mixed liquor comprising egg oil and lecithin from yolk；
（2）By step（1）Vacuum-concentrcted is to paste under the conditions of 30-35 DEG C for obtained mixed liquor, further 45
It is dried in vacuo, crushes under the conditions of DEG C, obtains powdered lecithins mixture；
（3）By step（2）Obtained powdered lecithins mixture adds extraction kettle, is passed through liquid carbon dioxide and carries out super face
Boundary extracts egg oil, and carbon dioxide is sent into separator with egg oil fluid-mixing, and further pressure release causes carbon dioxide and yolk
Oil is rapidly separated, and reclaims egg oil；Collected in extraction kettle and obtain lecithin crude product；
（4）In step（3）The ethanol that volumetric concentration is 85% is added in obtained lecithin crude product, controls amount of alcohol added,
Viscosity 10cP solution is mixed to get with lecithin crude product, then adds Aluminium Sulphate usp (powder), makes the lecithin in lecithin crude product
The emulsion system formed with neutral fats such as minimal amount of triglycerides, cholesterol destroys；Aluminum sulfate addition is lecithin crude product
The 4% of solution quality.
（5）Temperature is further reduced, carries out two-stage centrifugal processing：
The first order：Under the conditions of -30 DEG C with 2000rpm centrifugal speed under centrifuge, by minimal amount of based on cholesterol
Neutral fats except de-, obtain clear liquid；
The second level：The clear liquid that the first order is obtained is centrifuged under the conditions of -50 DEG C with 4000rpm centrifugal speed, will be few
The neutral fats based on triglycerides courage of amount is except de-；
（6）By step（5）By the solution that two-stage centrifugal obtains by being dried under reduced pressure, washing, ethyl acetate is washed, decompression is done
It is dry to obtain refined high-purity egg yolk lecithin.
By being examined to the fine egg yolk lecithin of collection, product purity has reached 98.1%.
Embodiment 4
（1）The duck's egg of low temperature storage is cleaned, ultraviolet sterilization is carried out, yolk is isolated under whole vacuum condition, by egg
The ethanol that yellow and volumetric concentration is 90% is with volume ratio 1:5 add high speed dispersor, and high speed dispersor temperature is constant at 15-20 DEG C,
It is scattered at a high speed with 5000rpm rotating speed, the lecithin in yolk is kept completely separate with egg yolk protein, jitter time 45min, so
After stand 15min, ethanol extracts the mixed liquor comprising egg oil and lecithin from yolk；
（2）By step（1）Vacuum-concentrcted is to paste under the conditions of 30-35 DEG C for obtained mixed liquor, further 45
It is dried in vacuo, crushes under the conditions of DEG C, obtains powdered lecithins mixture；
（3）By step（2）Obtained powdered lecithins mixture adds extraction kettle, is passed through liquid carbon dioxide and carries out super face
Boundary extracts egg oil, and carbon dioxide is sent into separator with egg oil fluid-mixing, and further pressure release causes carbon dioxide and yolk
Oil is rapidly separated, and reclaims egg oil；Collected in extraction kettle and obtain lecithin crude product；
（4）In step（3）The ethanol that volumetric concentration is 85% is added in obtained lecithin crude product, controls amount of alcohol added,
Viscosity 15cP solution is mixed to get with lecithin crude product, the mixture of alum and aluminum sulfate is then added, makes lecithin
The emulsion system that the neutral fats such as lecithin and minimal amount of triglycerides, cholesterol in crude product are formed destroys；Sulfate mixes
Thing addition is the 5% of lecithin crude product solution quality.
（5）Temperature is further reduced, carries out two-stage centrifugal processing：
The first order：Under the conditions of -30 DEG C with 25000rpm centrifugal speed under centrifuge, by minimal amount of based on cholesterol
Neutral fats except de-, obtain clear liquid；
The second level：The clear liquid that the first order is obtained is centrifuged under the conditions of -50 DEG C with 4500rpm centrifugal speed, will be few
The neutral fats based on triglycerides courage of amount is except de-；
（6）By step（5）By the solution that two-stage centrifugal obtains by being dried under reduced pressure, washing, ethyl acetate is washed, decompression is done
It is dry to obtain refined high-purity egg yolk lecithin.
By being examined to the fine egg yolk lecithin of collection, product purity has reached 98.3%.
Claims (6)
- A kind of 1. method by the purifying high-purity egg yolk lecithin that is demulsified, it is characterised in that：Specific extracting method is as follows：（1）By low temperature store egg washing, carry out ultraviolet sterilization, isolate yolk under whole vacuum condition, by yolk with Volumetric concentration is 90-95% ethanol with volume ratio 1:5-10 adds high speed dispersor, and high speed dispersor temperature is constant in 15-20 DEG C, it is scattered at a high speed with 5000-10000rpm rotating speed, the lecithin in yolk is kept completely separate with egg yolk protein, when disperseing Between 30-45min, then stand 15min, ethanol extracts the mixed liquor comprising egg oil and lecithin from yolk；（2）By step（1）Vacuum-concentrcted is to paste under the conditions of 30-35 DEG C for obtained mixed liquor, further in 45 DEG C of bars It is dried in vacuo, crushes under part, obtains powdered lecithins mixture；（3）By step（2）Obtained powdered lecithins mixture adds extraction kettle, is passed through liquid carbon dioxide and carries out overcritical extraction Egg oil is taken, carbon dioxide is sent into separator with egg oil fluid-mixing, and further pressure release make it that carbon dioxide is fast with egg oil Speed separation, reclaims egg oil；Collected in extraction kettle and obtain lecithin crude product；（4）In step（3）The ethanol that volumetric concentration is 80-85% is added in obtained lecithin crude product, controls amount of alcohol added, Viscosity 10-15cP solution is mixed to get with lecithin crude product, then adds sulfate, make lecithin in lecithin crude product with The emulsion system that the neutral fats such as minimal amount of triglycerides, cholesterol are formed destroys；Described sulfate is at least one of aluminum sulfate, alum；（5）Temperature is further reduced, carries out two-stage centrifugal processing：The first order：Under the conditions of -30 DEG C with 2000-3000rpm centrifugal speed under centrifuge, by minimal amount of based on cholesterol Neutral fats except de-, obtain clear liquid；The second level：The clear liquid that the first order is obtained is centrifuged under the conditions of -50 DEG C with 4000-5000rpm centrifugal speed, will be few The neutral fats based on triglycerides courage of amount is except de-；（6）By step（5）By the solution that two-stage centrifugal obtains by being dried under reduced pressure, washing, ethyl acetate is washed, is dried under reduced pressure To refined high-purity egg yolk lecithin.
- A kind of 2. method by the purifying high-purity egg yolk lecithin that is demulsified according to claim 1, it is characterised in that：Step （4）Described sulfate addition is the 3-5% of lecithin crude product solution quality.
- A kind of 3. method by the purifying high-purity egg yolk lecithin that is demulsified according to claim 1, it is characterised in that：Step （4）Described sulfate is the fine powder that particle diameter is less than 5 microns.
- A kind of 4. method by the purifying high-purity egg yolk lecithin that is demulsified according to claim 1, it is characterised in that：Step （4）Described sulfate is nanometer grade powder.
- A kind of 5. method by the purifying high-purity egg yolk lecithin that is demulsified according to claim 1, it is characterised in that：Step （5）Described first order centrifugal speed is 2500rpm.
- A kind of 6. method by the purifying high-purity egg yolk lecithin that is demulsified according to claim 1, it is characterised in that：Step （5）Described second level centrifugal speed is 4500rpm.
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