CN106632457A - Method for refining high-purity egg yolk lecithin through demulsification - Google Patents

Abstract

The invention belongs to the technical field of medical raw material processing, and in particular relates to a method for refining high-purity egg yolk lecithin through demulsification. This method is to further refine the lecithin crude product obtained through ethanol extraction and supercritical carbon dioxide extraction. The emulsion system formed by the neutral lipid is destroyed, so that the lecithin in the crude lecithin and the neutral lipid appear phase separation, further through the secondary cooling, a very small amount of triglyceride, cholesterol and other neutral lipids are removed under high-speed centrifugation conditions Removal, thereby refining high-purity egg yolk lecithin. The purity of the product is increased to more than 98%, realizing the clean and pollution-free production of high-purity egg yolk lecithin, fully satisfying the use of lecithin products as medicinal raw materials.

Description

A method for refining high-purity egg yolk lecithin by demulsification

technical field

The invention belongs to the technical field of medical raw material processing, and in particular relates to a method for refining high-purity egg yolk lecithin through demulsification.

Background technique

Lecithin is the basic substance of life, exists in every cell, is an important component of nerve tissue, and belongs to advanced nerve nutrients. Therefore, supplementing lecithin can activate brain cells, eliminate fatigue, enhance memory, and improve mental state, thereby maintaining the health of brain tissue and nervous system. In view of the special function of lecithin, it has gradually shifted from health care products to medicines. Because of its strong emulsifying effect on lipids, it can dissolve cholesterol, triglycerides, etc., so it has a significant effect on reducing lipids in blood vessel walls and inhibiting atherosclerosis.

In order to be more suitable for medicinal use, egg yolk lecithin with better biological activity and human utilization has become a key research object. Although there are many methods for extracting egg yolk lecithin at present, the purity is relatively low, and it is difficult to meet the requirements for use. The traditional method of extracting egg yolk lecithin generally uses an organic solvent method, and the obtained egg yolk lecithin is enriched in cholesterol, etc., so the purity is low, and the solvent is usually acetone, which introduces toxic and harmful solvents, which will not only cause organic solvents in the product residues and cause environmental pollution.

Chinese invention patent CN101029057A discloses a method for preparing egg yolk lecithin. This method uses poultry eggs as raw materials, separates egg yolk and stirs it into egg yolk liquid, extracts with edible alcohol, separates the extract, concentrates the extract, and dehydrates to obtain eggs The primary product of phospholipid is subjected to supercritical CO2 extraction on the primary product of lecithin to remove neutral fat to obtain lecithin from which neutral fat has been removed, but the purity of egg yolk lecithin obtained by this method still cannot meet the requirements for medical use.

Chinese invention patent CN1733777A discloses a preparation method of high-purity egg yolk lecithin, including 1) fresh egg yolk is first degreased with acetone, vacuum filtered, the filter cake is extracted with alcohol, the filtrate is combined, and vacuum concentrated to obtain crude phospholipid; 2) blunt 3) Crude phospholipids were dissolved in methanol and added to the chromatographic column, and the effluent was collected; 4) After the lecithin began to penetrate, rinse with pure methanol and collect effluent. Degreasing with acetone causes toxic residues and pollutes the environment.

Chinese invention patent CN102924506 A discloses a method for preparing high-purity lecithin, using simulated moving bed continuous chromatographic separation technology to ensure the effective separation of lecithin and other components contained in the raw material lipids to obtain high-purity lecithin products. The method is complicated in process, and although the purity is high, the efficiency is low, and it is difficult to meet the requirements of large-scale extraction.

For this reason, pollution-free, efficient and large-scale extraction of high-purity egg yolk lecithin is of great significance to the development of medicinal lecithin, but the prior art cannot fully meet the above-mentioned needs.

Contents of the invention

Aiming at the defect that the current egg yolk lecithin refining process is complex and easily causes secondary pollution, the present invention proposes a method for refining high-purity egg yolk lecithin through demulsification. Its outstanding feature is that lecithin has a strong emulsifying ability for neutral fats such as triglycerides and cholesterol, and it is difficult to separate lecithin from neutral fats such as triglycerides and cholesterol in crude lecithin. Demulsification, to separate a very small amount of triglyceride, cholesterol and other neutral fats in the crude lecithin, thus realizing the clean and pollution-free production of high-purity egg yolk lecithin. The obtained lecithin has a purity of more than 98%, which fully meets the lecithin product used as a medicinal raw material.

In order to achieve the above object, the present invention adopts the following technical solutions:

A method for refining high-purity egg yolk lecithin through demulsification, characterized in that: the specific extraction method is as follows:

(1) Clean the poultry eggs stored at low temperature, sterilize them with ultraviolet rays, separate the egg yolks under full vacuum conditions, add the egg yolks and ethanol with a volume concentration of 90-95% into the high-speed disperser at a volume ratio of 1:5-10, The temperature of the high-speed disperser is kept constant at 15-20°C, and the speed of 5000-10000rpm is used to disperse at a high speed, so that the lecithin in the egg yolk is completely separated from the egg yolk protein. The dispersion time is 30-45min, and then it is left for 15min. A mixture of egg yolk and lecithin;

(2) Concentrating the mixed solution obtained in step (1) under reduced pressure at 30-35°C to a paste, and further drying and pulverizing under vacuum at 45°C to obtain a powdery lecithin mixture;

(3) Put the powdery lecithin mixture obtained in step (2) into the extraction kettle, and feed liquid carbon dioxide to carry out supercritical extraction of egg yolk, and the mixed fluid of carbon dioxide and egg yolk is sent to the separator, and the pressure is further released so that the carbon dioxide and egg yolk are rapidly extracted. Separation and recovery of egg oil; collection of crude lecithin in the extraction kettle;

(4) Add ethanol with a volume concentration of 80-85% to the lecithin crude product obtained in step (3), control the amount of ethanol added, mix with the lecithin crude product to obtain a solution with a viscosity of 10-15cP, and then add sulfate to make the egg The emulsion system formed by the lecithin in the crude phospholipid and a very small amount of triglyceride, cholesterol and other neutral lipids is destroyed;

(5) Further lower the temperature and perform secondary centrifugation:

The first stage: Centrifuge at a centrifugal speed of 2000-3000rpm under the condition of -30°C to remove a very small amount of neutral lipids mainly including cholesterol to obtain a supernatant;

The second stage: Centrifuge the supernatant liquid obtained in the first stage at -50°C at a centrifugal speed of 4000-5000rpm to remove a very small amount of neutral fat mainly composed of triglyceride bile;

(6) The solution obtained in step (5) through secondary centrifugation is dried under reduced pressure, washed with water, washed with ethyl acetate, and dried under reduced pressure to obtain refined high-purity egg yolk lecithin.

Preferably, the sulfate described in step (4) is at least one of aluminum sulfate and aluminum potassium sulfate.

Preferably, the amount of sulfate added in step (4) is 3-5% of the mass of the crude lecithin solution.

Preferably, the sulfate described in step (4) is a fine powder with a particle size of less than 5 microns.

Further preferably, the sulfate described in step (4) is a nanoscale powder.

Preferably, the first-stage centrifugal speed in step (5) is 2500 rpm.

Preferably, the second-stage centrifugal speed in step (5) is 4500 rpm.

Because lecithin has a strong emulsifying ability to triglycerides and cholesterol, lecithin and neutral oils such as triglycerides and cholesterol exist in a homogeneous phase in the crude product of lecithin. Some egg oil, but a small amount of neutral oils such as triglycerides and cholesterol affect the quality of lecithin, resulting in low purity of lecithin, which cannot be used as a medical raw material.

The outstanding feature of the present invention is that the lecithin crude product obtained through ethanol extraction and supercritical carbon dioxide extraction is further refined, and its remarkable progress is that sulfate is used to make the lecithin in the lecithin crude product and a very small amount of triglyceride The emulsion system formed by neutral lipids such as cholesterol and cholesterol is destroyed, so that the lecithin and neutral lipids in the crude lecithin are phase-separated, and further through secondary cooling, a very small amount of triglycerides, cholesterol, etc. Neutral fat is removed to refine high-purity egg yolk lecithin.

A typical operation example increases the purity of the product to more than 98%, realizes the clean and pollution-free production of high-purity egg yolk lecithin, and fully satisfies the use of lecithin products as medicinal raw materials. The more significant advantage is that ethyl acetate is used to wash the lecithin during the refining process, which effectively prevents the lecithin from being affected by the external oxygen and water environment, better ensures the activity of the lecithin, and prolongs its shelf life.

The present invention is a method for refining high-purity egg yolk lecithin through demulsification. Compared with the prior art, its outstanding features and excellent effects are as follows:

1. Sulfate is used to destroy the emulsion system formed by the lecithin in the crude lecithin and a very small amount of triglyceride, cholesterol and other neutral lipids, so that the lecithin and neutral lipids in the crude lecithin are phase-separated , further through two-stage cooling, a very small amount of triglycerides, cholesterol and other neutral fats are removed under high-speed centrifugation conditions, thereby refining high-purity egg yolk lecithin.

2. Washing with ethyl acetate during the refining process effectively prevents the lecithin from being affected by the external oxygen and water environment, better ensures the activity of the lecithin and prolongs its shelf life.

3. The preparation method provided by the present invention realizes the clean and pollution-free production of high-purity egg yolk lecithin, which fully satisfies the use of lecithin products as medicinal raw materials.

detailed description

The present invention will be further explained by specific examples below, but it should not be understood that the scope of the present invention is limited to the following examples. Without departing from the above-mentioned method idea of the present invention, various replacements or changes made according to common technical knowledge and customary means in this field shall be included in the scope of the present invention.

Example 1

(1) Wash the eggs stored at low temperature, sterilize them by ultraviolet light, separate the egg yolk under the whole vacuum condition, add the egg yolk and ethanol with a volume concentration of 95% to the high-speed disperser at a volume ratio of 1:5, and the temperature of the high-speed disperser is constant At 15-20°C, disperse at a high speed of 5000rpm to completely separate the lecithin in the egg yolk from the egg yolk protein. The dispersion time is 30 minutes, and then stand for 15 minutes. Ethanol extracts a mixture containing egg yolk and lecithin from the egg yolk;

(2) Concentrating the mixed solution obtained in step (1) under reduced pressure at 30-35°C to a paste, and further drying and pulverizing under vacuum at 45°C to obtain a powdery lecithin mixture;

(3) Put the powdery lecithin mixture obtained in step (2) into the extraction kettle, and feed liquid carbon dioxide to carry out supercritical extraction of egg yolk, and the mixed fluid of carbon dioxide and egg yolk is sent to the separator, and the pressure is further released so that the carbon dioxide and egg yolk are rapidly extracted. Separation and recovery of egg oil; collection of crude lecithin in the extraction kettle;

(4) Add ethanol with a volume concentration of 80% to the lecithin crude product obtained in step (3), control the amount of ethanol added, mix with the lecithin crude product to obtain a solution with a viscosity of 10 cP, and then add aluminum sulfate powder with a particle size of less than 5 μm, The emulsion system formed by the lecithin in the crude lecithin and a very small amount of neutral lipids such as triglyceride and cholesterol is destroyed by stirring; the amount of aluminum sulfate added is 3% of the mass of the crude lecithin solution.

(5) Further lower the temperature and perform secondary centrifugation:

The first stage: Centrifuge at -30°C at a centrifugal speed of 2500rpm to remove a very small amount of neutral lipids mainly including cholesterol to obtain a supernatant;

The second stage: Centrifuge the supernatant liquid obtained in the first stage at -50°C at a centrifugal speed of 4500rpm to remove a very small amount of neutral fat mainly composed of triglyceride bile;

(6) The solution obtained in step (5) through secondary centrifugation is dried under reduced pressure, washed with water, washed with ethyl acetate, and dried under reduced pressure to obtain refined high-purity egg yolk lecithin.

Through the inspection of the collected fine egg yolk lecithin, the product purity reaches 98.5%.

Example 2

(1) Wash the goose eggs stored at low temperature, sterilize them with ultraviolet light, separate the egg yolk under the whole vacuum condition, add the egg yolk and ethanol with a volume concentration of 95% to the high-speed disperser at a volume ratio of 1:8, and the temperature of the high-speed disperser Constantly at 15-20°C, disperse at a high speed of 10000rpm to completely separate the lecithin in the egg yolk from the egg yolk protein. The dispersion time is 45 minutes, and then stand for 15 minutes. Ethanol extracts a mixture containing egg yolk and lecithin from the egg yolk ;

(2) Concentrating the mixed solution obtained in step (1) under reduced pressure at 30-35°C to a paste, and further drying and pulverizing under vacuum at 45°C to obtain a powdery lecithin mixture;

(3) Put the powdery lecithin mixture obtained in step (2) into the extraction kettle, and feed liquid carbon dioxide to carry out supercritical extraction of egg yolk, and the mixed fluid of carbon dioxide and egg yolk is sent to the separator, and the pressure is further released so that the carbon dioxide and egg yolk are rapidly extracted. Separation and recovery of egg oil; collection of crude lecithin in the extraction kettle;

(4) adding volume concentration to the lecithin crude product obtained in step (3) is 85% ethanol, controlling the amount of ethanol added, mixing with the lecithin crude product to obtain a solution with a viscosity of 15cP, then adding potassium aluminum sulfate nanopowder to make the lecithin The emulsion system formed by the lecithin in the crude product and a very small amount of triglyceride, cholesterol and other neutral fats is destroyed; the addition of potassium aluminum sulfate is 5% of the mass of the lecithin crude product solution.

(5) Further lower the temperature and perform secondary centrifugation:

The first stage: Centrifuge at -30°C at a centrifugal speed of 3000rpm to remove a very small amount of neutral lipids mainly including cholesterol to obtain a supernatant;

The second stage: Centrifuge the supernatant liquid obtained in the first stage at -50°C at a centrifugal speed of 5000rpm to remove a very small amount of neutral fat mainly composed of triglyceride bile;

(6) The solution obtained in step (5) through secondary centrifugation is dried under reduced pressure, washed with water, washed with ethyl acetate, and dried under reduced pressure to obtain refined high-purity egg yolk lecithin.

Through the routine detection of the collected fine egg yolk lecithin, its composition is: phosphatidylcholine 98.0%, phosphatidylethanolamine 0.5%, lysophosphatidylcholine 0.5%.

Example 3

(1) Wash the quail eggs stored at low temperature, sterilize them with ultraviolet rays, separate the egg yolk under the whole vacuum condition, add the egg yolk and ethanol with a volume concentration of 90% to the high-speed disperser at a volume ratio of 1:10, and the temperature of the high-speed disperser Constantly at 15-20°C, disperse at a high speed of 8000rpm to completely separate the lecithin in the egg yolk from the egg yolk protein. The dispersion time is 30 minutes, and then stand for 15 minutes. Ethanol extracts the mixture containing egg yolk and lecithin from the egg yolk ;

(2) Concentrating the mixed solution obtained in step (1) under reduced pressure at 30-35°C to a paste, and further drying and pulverizing under vacuum at 45°C to obtain a powdery lecithin mixture;

(3) Put the powdery lecithin mixture obtained in step (2) into the extraction kettle, and feed liquid carbon dioxide to carry out supercritical extraction of egg yolk, and the mixed fluid of carbon dioxide and egg yolk is sent to the separator, and the pressure is further released so that the carbon dioxide and egg yolk are rapidly extracted. Separation and recovery of egg oil; collection of crude lecithin in the extraction kettle;

(4) Add ethanol with a volume concentration of 85% to the lecithin crude product obtained in step (3), control the amount of ethanol added, mix with the lecithin crude product to obtain a solution with a viscosity of 10 cP, and then add aluminum sulfate powder to make the lecithin crude product The emulsion system formed by the lecithin and a very small amount of triglyceride, cholesterol and other neutral fats is destroyed; the addition of aluminum sulfate is 4% of the mass of the crude lecithin solution.

(5) Further lower the temperature and perform secondary centrifugation:

The first stage: Centrifuge at -30°C at a centrifugal speed of 2000rpm to remove a very small amount of neutral lipids mainly including cholesterol to obtain a supernatant;

The second stage: Centrifuge the supernatant liquid obtained in the first stage at -50°C at a centrifugal speed of 4000rpm to remove a very small amount of neutral fat mainly composed of triglyceride bile;

(6) The solution obtained in step (5) through secondary centrifugation is dried under reduced pressure, washed with water, washed with ethyl acetate, and dried under reduced pressure to obtain refined high-purity egg yolk lecithin.

Through the inspection of the collected fine egg yolk lecithin, the product purity reaches 98.1%.

Example 4

(1) Wash the duck eggs stored at low temperature, sterilize them with ultraviolet rays, separate the egg yolk under the whole vacuum condition, add the egg yolk and ethanol with a volume concentration of 90% to the high-speed disperser at a volume ratio of 1:5, and the temperature of the high-speed disperser is constant At 15-20°C, disperse at a high speed of 5000rpm to completely separate the lecithin in the egg yolk from the egg yolk protein. The dispersion time is 45 minutes, and then stand for 15 minutes. Ethanol extracts a mixture containing egg yolk and lecithin from the egg yolk;

(2) Concentrating the mixed solution obtained in step (1) under reduced pressure at 30-35°C to a paste, and further drying and pulverizing under vacuum at 45°C to obtain a powdery lecithin mixture;

(3) Put the powdery lecithin mixture obtained in step (2) into the extraction kettle, and feed liquid carbon dioxide to carry out supercritical extraction of egg yolk, and the mixed fluid of carbon dioxide and egg yolk is sent to the separator, and the pressure is further released so that the carbon dioxide and egg yolk are rapidly extracted. Separation and recovery of egg oil; collection of crude lecithin in the extraction kettle;

(4) adding ethanol with a volume concentration of 85% to the lecithin crude product obtained in step (3), controlling the amount of ethanol added, mixing with the lecithin crude product to obtain a solution with a viscosity of 15cP, then adding the mixture of potassium aluminum sulfate and aluminum sulfate, Destroy the emulsion system formed by the lecithin in the crude lecithin and a very small amount of triglyceride, cholesterol and other neutral lipids; the amount of the sulfate mixture added is 5% of the mass of the crude lecithin solution.

(5) Further lower the temperature and perform secondary centrifugation:

The first stage: Centrifuge at -30°C at a centrifugal speed of 25,000 rpm to remove a very small amount of neutral lipids mainly consisting of cholesterol to obtain a supernatant;

The second stage: Centrifuge the supernatant liquid obtained in the first stage at -50°C at a centrifugal speed of 4500rpm to remove a very small amount of neutral fat mainly composed of triglyceride bile;

(6) The solution obtained in step (5) through secondary centrifugation is dried under reduced pressure, washed with water, washed with ethyl acetate, and dried under reduced pressure to obtain refined high-purity egg yolk lecithin.

Through the inspection of the collected fine egg yolk lecithin, the product purity reaches 98.3%.

Claims (7)

1. a kind of method by breakdown of emulsion purifying high-purity egg yolk lecithin, it is characterised in that：Concrete 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 the ethanol of 90-95% with volume ratio 1:5-10 adds high speed dispersor, and high speed dispersor temperature constant is in 15-20 DEG C, disperseed at a high speed with the rotating speed of 5000-10000rpm, the lecithin in yolk is kept completely separate with egg yolk protein, during dispersion Between 30-45min, then stand 15min, ethanol extracts the mixed liquor comprising egg oil and lecithin from yolk；

（2）By step（1）The mixed liquor for obtaining under the conditions of 30-35 DEG C vacuum-concentrcted to paste, further in 45 DEG C of bars Vacuum drying, crushing, obtain powdered lecithins mixture under part；

（3）By step（2）The powdered lecithins mixture for obtaining adds extraction kettle, and being passed through liquid carbon dioxide carries out overcritical extraction Egg oil is taken, carbon dioxide sends into separator with egg oil fluid-mixing, and further pressure release causes carbon dioxide fast with egg oil Speed is separated, and reclaims egg oil；Collect in extraction kettle and obtain lecithin crude product；

（4）In step（3）Add volumetric concentration for the ethanol of 80-85% in the lecithin crude product for obtaining, control amount of alcohol added, Solution with lecithin crude product is mixed to get viscosity 10-15cP, is subsequently adding sulfate, make lecithin in lecithin crude product with The emulsion system destruction that the neutral fats such as minimal amount of triglycerides, cholesterol are formed；

（5）Temperature is further reduced, two-stage centrifugal process is carried out：

The first order：To be centrifuged under the centrifugal speed of 2000-3000rpm under the conditions of -30 DEG C, 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 the centrifugal speed of 4000-5000rpm, will be few The neutral fats based on triglycerides courage of amount is except de-；

（6）By step（5）The solution obtained through two-stage centrifugal is washed by drying under reduced pressure, washing, ethyl acetate, drying under reduced pressure is obtained To refined high-purity egg yolk lecithin.

2. a kind of method by breakdown of emulsion purifying high-purity egg yolk lecithin according to claim 1, it is characterised in that：Step （4）Described sulfate is at least one in aluminum sulfate, alum.

3. a kind of method by breakdown of emulsion purifying high-purity egg yolk lecithin according to claim 1, it is characterised in that：Step （4）Described sulfate addition is the 3-5% of lecithin crude product solution quality.

4. a kind of method by breakdown of emulsion purifying high-purity egg yolk lecithin according to claim 1, it is characterised in that：Step （4）Described sulfate is fine powder of the particle diameter less than 5 microns.

5. a kind of method by breakdown of emulsion purifying high-purity egg yolk lecithin according to claim 1, it is characterised in that：Step （4）Described sulfate is nanometer grade powder.

6. a kind of method by breakdown of emulsion purifying high-purity egg yolk lecithin according to claim 1, it is characterised in that：Step （5）Described first order centrifugal speed is 2500rpm.

7. a kind of method by breakdown of emulsion purifying high-purity egg yolk lecithin according to claim 1, it is characterised in that：Step （5）Described second level centrifugal speed is 4500rpm.