CN110938091B - High-efficiency extraction method of egg yolk lecithin - Google Patents
High-efficiency extraction method of egg yolk lecithin Download PDFInfo
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- 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 System
- 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
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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
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- 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
An efficient extraction method of yolk lecithin, belonging to the technical field of biomedical raw material processing. Taking liquid egg yolk as a raw material, treating egg yolk liquid by adopting subcritical carbon dioxide fluid, separating egg yolk oil, and completing degreasing; then carrying out vacuum freeze drying on the degreased egg yolk liquid to obtain egg yolk powder; and finally, extracting and purifying the yolk powder by using supercritical carbon dioxide fluid to obtain the yolk lecithin. The method is safe and environment-friendly, and the obtained product has high activity, good quality and no solvent residue, and has great application potential in the pharmaceutical and food industries.
Description
Technical Field
The invention belongs to the technical field of biomedical raw material processing, and particularly relates to a high-efficiency extraction method of egg yolk lecithin.
Background
Yolk lecithin, also known as yolk essence, has physiological functions of regulating blood fat, promoting brain development, enhancing memory and the like, and plays an important role in the pharmaceutical industry. At present, the extraction from egg yolk is the main method for producing egg yolk lecithin, but the egg yolk lecithin has poor stability and is easy to oxidize, the correlation degree of the activity and the temperature is very high, and the activity is basically lost when the temperature exceeds 50 ℃. Therefore, high requirements are put on the extraction technology and the process of the egg yolk lecithin.
At present, the method for extracting yolk lecithin from yolk generally adopts organic solvent extraction and supercritical CO 2 An extraction method. The invention patent CN 106632457A discloses a method for refining high-purity egg yolk lecithin through demulsification, which is characterized in that egg yolk is subjected to ethanol extraction and supercritical carbon dioxide extraction to obtain an egg yolk lecithin crude product, the egg yolk lecithin crude product is further refined, a sulfate damage emulsion system is introduced, and the obtained product has the purity of 98% through refining processes such as phase separation, secondary cooling, high-speed centrifugation and the like. The invention patent CN 106632458B provides a method for yolk lecithin, which also adopts ethanol to extract yolk and takes supernatant fluid to obtain a yolk lecithin crude product, and then the yolk lecithin crude product is obtained through decompression concentration and vacuum freeze drying; and (3) grinding the crude product into fine particles by air flow under the protection of nitrogen, and then performing two-stage extraction process by a supercritical extraction kettle with a variable-frequency magnetizing device to obtain the egg yolk lecithin through separation and collection. In the methods, the organic reagent is used as a carrying agent or an extracting agent, so that the method is not beneficial to environmental protection and is easy to generate the problem of solvent residue; extraction process routeThe method is complex, the temperature in the extraction process is relatively high, and the biological activity of the extracted product is low; in addition, the separation efficiency of egg yolk oil and egg yolk lecithin is low, and the extraction rate of egg yolk lecithin is low.
Disclosure of Invention
The invention provides a high-efficiency extraction method of egg yolk lecithin, which has high product activity, high extraction rate, safety and environmental protection and aims at solving the problems of organic solvent residue, low extraction rate and poor activity of extracted products commonly existing in the extraction process.
In order to achieve the purpose, the invention discloses a high-efficiency extraction method of yolk lecithin, which comprises the following steps: taking liquid egg yolk as a raw material, treating egg yolk liquid by adopting subcritical carbon dioxide fluid, separating egg yolk oil, and completing degreasing; then carrying out vacuum freeze drying on the degreased egg yolk liquid to obtain egg yolk powder; and finally, extracting and purifying the yolk powder by using supercritical carbon dioxide fluid to obtain the yolk lecithin.
Preferably, the specific operation of treating the egg yolk liquid by using the subcritical carbon dioxide fluid is as follows: feeding the yolk liquid into an extraction device, introducing carbon dioxide, maintaining the temperature at 25-30 deg.C, and extracting under 6-8 MPa for 2-4 hr to obtain yolk oil and defatted yolk liquid.
Preferably, the subcritical carbon dioxide treatment is carried out under the conditions of pressure 8MPa, temperature 30 ℃ and time 2h.
Preferably, the specific operation of the vacuum freeze drying to obtain the egg yolk powder is as follows:
placing the degreased egg yolk liquid in a vacuum freeze dryer, wherein the thickness of the egg yolk liquid is 4-6 mm; cooling to-40 to-30 ℃ at the speed of 10 ℃/min, and keeping for 2 to 4 hours; then starting a vacuum pump, adjusting the vacuum degree to 30-60 Pa, and drying for 6-8 h; and finally, heating to 30-45 ℃, keeping the temperature of the cold trap at minus 40-minus 35 ℃, and continuously keeping for 1-2 hours to obtain the egg yolk powder.
Preferably, the egg yolk liquid has a thickness of 4mm; the temperature reduction is carried out at-35 ℃ for 3h; the vacuum degree is 50Pa, and the drying is carried out for 8 hours; the temperature rise is 40 ℃, the temperature of the cold trap is-35 ℃, and the drying is carried out for 2 hours.
Preferably, the specific steps of extracting and purifying the yolk powder by using the supercritical carbon dioxide fluid are as follows: adding yolk powder into an extraction kettle, setting the extraction temperature to be 25-30 ℃, introducing liquid carbon dioxide for supercritical extraction, and extracting for 2-3 h under the pressure of 15-18 MPa; then decompressing to 5MPa-6MPa, separating at 25 deg.C to obtain egg yolk lecithin.
Preferably, the supercritical extraction conditions comprise that the extraction temperature is 30 ℃, the extraction pressure is 18MPa, and the extraction time is 2 hours; the separation conditions were a pressure of 5MPa and a temperature of 25 ℃.
On the other hand, the invention discloses the yolk lecithin prepared by the extraction method.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the method adopts the subcritical carbon dioxide, vacuum freeze drying and supercritical carbon dioxide to extract the egg yolk lecithin in the egg yolk, the egg yolk oil is completely extracted, the egg yolk lecithin is fully released, the purity of the finally obtained egg yolk oil and the purity of the egg yolk lecithin are both more than 95%, and the extraction rate is more than 85%.
2. Under the subcritical carbon dioxide state, the extract is in a soaking state, the short circuit and bonding phenomena of a feed liquid layer can be avoided, meanwhile, the grease, cholesterol and the like in the egg yolk can be efficiently and thoroughly removed, the drying and extraction efficiency and purity of the egg yolk lecithin can be improved, the extraction time is shortened, the extraction pressure is reduced, the production efficiency is improved, and the method is suitable for industrial production.
3. The invention adopts subcritical and supercritical carbon dioxide fluid extraction method, abandons the use of traditional organic solvent, and the obtained product has no solvent residue, and is safe and environment-friendly.
4. The extraction process of the invention has the advantages that all steps are operated under low temperature condition, and the biological activity of the extracted product can be maintained to the maximum extent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a high-efficiency extraction method of yolk lecithin, which comprises the following steps: fresh liquid egg yolk is used as a raw material, subcritical carbon dioxide fluid is adopted to treat egg yolk liquid, egg yolk oil is separated, and degreasing is completed; then carrying out vacuum freeze drying on the degreased egg yolk liquid to obtain egg yolk powder; and finally, extracting and purifying the yolk powder by using supercritical carbon dioxide fluid to obtain the yolk lecithin.
In the above embodiments, the method of subcritical carbon dioxide, vacuum freeze drying and supercritical carbon dioxide is adopted to extract the egg yolk lecithin from the egg yolk, the egg yolk oil is completely extracted, the egg yolk lecithin is fully released, the purity of the obtained egg yolk oil and the purity of the obtained egg yolk lecithin are both above 95%, and the extraction rate is both above 85%.
In an alternative embodiment, the specific operation of the subcritical carbon dioxide fluid treatment of egg yolk liquid is as follows: feeding the yolk liquid into an extraction device, introducing carbon dioxide, maintaining the temperature at 25-30 deg.C, and extracting under 6-8 MPa for 2-4 hr to obtain yolk oil and defatted yolk liquid. In the embodiment, the carbon dioxide has special thermal property and transmission characteristic in the subcritical state, has relative stability and rapidity, has small damage to effective components with poor heat sensitivity, can efficiently and completely remove grease, cholesterol and the like in egg yolk, and is beneficial to improving the drying and extraction efficiency and purity of egg yolk lecithin.
In an optional embodiment, the vacuum freeze drying is carried out to obtain the yolk powder, wherein the method comprises the following specific steps of putting degreased yolk liquid into a vacuum freeze dryer, wherein the thickness of the yolk liquid is 4mm-6mm, cooling to-40 ℃ to-30 ℃ at the speed of 10 ℃/min, and keeping for 2h-4h; then starting a vacuum pump, adjusting the vacuum degree to 30-60 Pa, and drying for 6-8 h; and finally, heating to 30-45 ℃, keeping the temperature of the cold trap at minus 40-minus 35 ℃, and continuously keeping for 2 hours to obtain the egg yolk powder.
In the above embodiments, the egg yolk liquid is degreased and then the egg yolk powder is prepared by a vacuum freeze drying method, and the obtained egg yolk powder has bright color, is loose and porous, has regular granularity, and is beneficial to extracting egg yolk lecithin. And finally heating to 30-45 ℃ in the process, drying for 2h, wherein the temperature is too low to be beneficial to removing water, the temperature is too high to destroy the biological activity of the product, and under the condition of 30-45 ℃, the complete biological activity of the egg yolk lecithin can be maintained while ensuring that the water which is not frozen is rapidly removed.
In an alternative embodiment, the specific steps of extracting and purifying the yolk powder by using the supercritical carbon dioxide fluid are as follows: adding yolk powder into an extraction kettle, setting the extraction temperature to be 25-30 ℃, introducing liquid carbon dioxide for supercritical extraction, and extracting for 2-3 h under the pressure of 15-18 MPa; then decompressing to 5MPa-6MPa, separating at 25 deg.C to obtain egg yolk lecithin. In the embodiment, due to the degreasing and drying processes of the previous working procedures, the yolk powder is loose and porous and has regular granularity, and the release of the yolk lecithin is facilitated, so that the extraction of the yolk lecithin can be realized under the pressure of 15-18 MPa; in addition, the product is separated by adopting an isothermal depressurization method, the solute is left in the extraction kettle, and the carbon dioxide gas returns to the extractor for recycling through a compressor.
In a preferred embodiment, the subcritical carbon dioxide treatment condition is that the pressure is 8MPa, the temperature is 30 ℃, and the time is 2h; the conditions of vacuum freeze-drying are as follows: cooling yolk liquid to-35 deg.C at a speed of 4mm,10 deg.C/min, maintaining for 3h, adjusting vacuum degree to 50Pa, drying for 8h, heating to 40 deg.C, and drying for 2h at-35 deg.C; the conditions of the supercritical extraction are as follows: the extraction temperature is 30 ℃, the extraction pressure is 18MPa, and the extraction time is 2h; the separation conditions were a pressure of 5MPa and a temperature of 25 ℃. Under the conditions of the above examples, the extraction rate of egg yolk lecithin was the highest, and the quality was the best.
The embodiment of the invention also discloses the yolk lecithin prepared by the extraction method. The yolk lecithin obtained in the embodiment has high purity and good activity, the purity (PC content) can reach 98 percent at most, and the yolk lecithin has great application potential in the pharmaceutical and food industries.
In order to more clearly and specifically describe the method for extracting egg yolk lecithin with high efficiency provided by the embodiment of the present invention, the following description will be made with reference to specific embodiments.
Example 1
Feeding fresh egg yolk liquid into an extraction device, introducing carbon dioxide, maintaining the temperature at 25 deg.C, and extracting under 6MPa for 2 hr to obtain egg yolk oil and defatted egg yolk liquid.
Placing the degreased egg yolk liquid in a vacuum freeze dryer, wherein the thickness of the egg yolk liquid is 4mm; cooling to-40 deg.C at a speed of 10 deg.C/min, and maintaining for 3 hr; then starting a vacuum pump, adjusting the vacuum degree to 36.5Pa, and drying for 8h; and finally, heating to 35 ℃, keeping the temperature of the cold trap at-40 ℃, and continuously keeping for 2 hours to obtain the egg yolk powder.
Adding yolk powder into an extraction kettle, setting the extraction temperature at 30 ℃, introducing liquid carbon dioxide for supercritical extraction, and extracting for 2h under the pressure of 18 MPa; then decompressing to 6MPa, separating at 25 ℃ to obtain the egg yolk lecithin.
Through detection: the purity of the egg yolk oil and the egg yolk lecithin is respectively 80 percent and 90 percent, and the extraction rate reaches 80 percent.
Example 2
Feeding fresh egg yolk liquid into an extraction device, introducing carbon dioxide, maintaining the temperature at 25 deg.C, and extracting under 8MPa for 2 hr to obtain egg yolk oil and defatted egg yolk liquid.
Placing the degreased egg yolk liquid in a vacuum freeze dryer, wherein the thickness of the egg yolk liquid is 4mm; cooling to-30 deg.C at a speed of 10 deg.C/min, and maintaining for 3 hr; then starting a vacuum pump, and adjusting the vacuum degree to 50Pa for drying for 8h; and finally, heating to 35 ℃, simultaneously keeping the temperature of the cold trap at-35 ℃, and continuously keeping for 2 hours to obtain the egg yolk powder.
Adding yolk powder into an extraction kettle, setting the extraction temperature at 30 ℃, introducing liquid carbon dioxide for supercritical extraction, and extracting for 2h under the pressure of 18 MPa; then decompressing to 6MPa, separating at 25 ℃ to obtain the egg yolk lecithin.
Through detection: the purity of the egg yolk oil and the egg yolk lecithin is respectively 90 percent and 95 percent, and the extraction rate is 85 percent.
Example 3
Feeding fresh egg yolk liquid into an extraction device, introducing carbon dioxide, maintaining the temperature at 30 deg.C, and extracting under 8MPa for 2 hr to obtain egg yolk oil and defatted egg yolk liquid.
Placing the degreased egg yolk liquid in a vacuum freeze dryer, wherein the thickness of the egg yolk liquid is 6mm; cooling to-40 deg.C at a speed of 10 deg.C/min, and maintaining for 2 hr; then starting a vacuum pump, adjusting the vacuum degree to 60Pa, and drying for 8h; and finally, heating to 45 ℃, simultaneously keeping the temperature of the cold trap at-35 ℃, and continuously keeping for 2 hours to obtain the egg yolk powder.
Adding yolk powder into an extraction kettle, setting the extraction temperature at 30 ℃, introducing liquid carbon dioxide for supercritical extraction, and extracting for 2h under the pressure of 18 MPa; then decompressing to 6MPa, separating at 25 ℃ to obtain the egg yolk lecithin.
And (3) detection: the egg yolk oil and egg yolk lecithin have purity of 85% and 92%, respectively, and extraction rate of 83%
Example 4
Feeding fresh egg yolk liquid into an extraction device, introducing carbon dioxide, maintaining the temperature at 30 deg.C, and extracting under 8MPa for 2 hr to obtain egg yolk oil and defatted egg yolk liquid.
Placing the degreased egg yolk liquid in a vacuum freeze dryer, wherein the thickness of the egg yolk liquid is 4mm; cooling to-35 deg.C at a speed of 10 deg.C/min, and maintaining for 3 hr; then starting a vacuum pump, and adjusting the vacuum degree to 50Pa for drying for 8h; and finally, heating to 40 ℃, keeping the temperature of the cold trap at-35 ℃, and continuously keeping for 2 hours to obtain the egg yolk powder.
Adding yolk powder into an extraction kettle, setting the extraction temperature at 30 ℃, introducing liquid carbon dioxide for supercritical extraction, and extracting for 2h under the pressure of 18 MPa; then decompressing to 5MPa, separating at 25 ℃ to obtain the egg yolk lecithin.
Through detection: the egg yolk oil and egg yolk lecithin have purity of 95% and 98%, respectively, and extraction rate of 85%
In conclusion, the method can quickly and efficiently extract the high-purity egg yolk lecithin, has high production efficiency and good product bioactivity, can obtain the high-purity egg yolk oil in the extraction process, and is very suitable for industrial production.
The list of examples set forth above is intended only as a comprehensive description of possible embodiments of the invention and is intended to impose any limitation on the scope of the invention, and equivalent embodiments or modifications made without departing from the technology of the invention are intended to be within the scope of the invention.
Claims (4)
1. The efficient extraction method of yolk lecithin is characterized in that liquid yolk is used as a raw material, subcritical carbon dioxide fluid is adopted to treat yolk liquid, yolk oil is separated out, and degreasing is finished; then carrying out vacuum freeze drying on the degreased egg yolk liquid to obtain egg yolk powder; finally, extracting and purifying the yolk powder by adopting supercritical carbon dioxide fluid to obtain yolk lecithin; the processes of degreasing and vacuum freeze drying enable the yolk powder to be loose and porous and have regular granularity, and the yolk powder is beneficial to the release of yolk lecithin; the obtained egg yolk oil and egg yolk lecithin have purity of more than 95% and extraction rate of more than 85%;
the specific operation of adopting the subcritical carbon dioxide fluid to treat the egg yolk liquid is as follows: feeding the yolk liquid into an extraction device, introducing carbon dioxide, maintaining the temperature at 25-30 deg.C, and extracting under 6-8 MPa for 2-4 hr to obtain yolk oil and defatted yolk liquid;
the specific operation of the vacuum freeze drying to obtain the egg yolk powder is as follows: placing the degreased egg yolk liquid in a vacuum freeze dryer, wherein the thickness of the egg yolk liquid is 4-6 mm; cooling to-40 to-30 ℃ at the speed of 10 ℃/min, and keeping for 2 to 4 hours; then starting a vacuum pump, adjusting the vacuum degree to 30-60 Pa, and drying for 6-8 h; finally, heating to 30-45 ℃, keeping the temperature of the cold trap at-40 ℃ to-35 ℃, and continuously keeping for 1-2 hours to obtain the egg yolk powder;
the method for extracting and purifying the egg yolk powder by using the supercritical carbon dioxide fluid comprises the following specific steps: adding yolk powder into an extraction kettle, setting the extraction temperature to be 25-30 ℃, introducing liquid carbon dioxide for supercritical extraction, and extracting for 2-3 h under the pressure of 15-18 MPa; then decompressing to 5MPa-6MPa, separating at 25 deg.C to obtain egg yolk lecithin.
2. The extraction process according to claim 1, wherein the subcritical carbon dioxide treatment is carried out under a pressure of 8MPa, at a temperature of 30 ℃ and for a period of 2 hours.
3. The extraction process according to claim 1, wherein the egg yolk liquid has a thickness of 4mm; the temperature reduction temperature is-35 ℃, and the temperature is kept for 3 hours; the vacuum degree is 50Pa, and the drying is carried out for 8 hours; the temperature rise is 40 ℃, the cold trap temperature is-35 ℃, and the temperature is kept for 2h.
4. The extraction method as claimed in claim 1, wherein the supercritical extraction conditions comprise an extraction temperature of 30 ℃, an extraction pressure of 18MPa, and an extraction time of 2h; the separation conditions were a pressure of 5MPa and a temperature of 25 ℃.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257660A (en) * | 1998-11-27 | 2000-06-28 | 克鲁普－犹德有限公司 | Method for obtaining, especially lecithine, from egg powder |
| CN1502619A (en) * | 2002-11-25 | 2004-06-09 | 石油大学(北京) | Method for separation preparing lecithine and apparatus using said method |
| WO2007123424A1 (en) * | 2006-04-20 | 2007-11-01 | Owen John Catchpole | Process for separating lipid materials |
| CN103706145A (en) * | 2012-10-01 | 2014-04-09 | 青岛科技大学 | Subcritical CO2 based method used for low-temperature removing of residual solvents from thermal sensitive solid medicines |
| CN107569868A (en) * | 2017-09-21 | 2018-01-12 | 珠海澳盈生物科技有限公司 | Using supercritical CO2The method for extracting de-fatted egg yolk powder |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257660A (en) * | 1998-11-27 | 2000-06-28 | 克鲁普－犹德有限公司 | Method for obtaining, especially lecithine, from egg powder |
| CN1502619A (en) * | 2002-11-25 | 2004-06-09 | 石油大学(北京) | Method for separation preparing lecithine and apparatus using said method |
| WO2007123424A1 (en) * | 2006-04-20 | 2007-11-01 | Owen John Catchpole | Process for separating lipid materials |
| CN103706145A (en) * | 2012-10-01 | 2014-04-09 | 青岛科技大学 | Subcritical CO2 based method used for low-temperature removing of residual solvents from thermal sensitive solid medicines |
| CN107569868A (en) * | 2017-09-21 | 2018-01-12 | 珠海澳盈生物科技有限公司 | Using supercritical CO2The method for extracting de-fatted egg yolk powder |
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