Egg yolk oil with anti-allergic effect and low-temperature extraction and purification process thereof

Abstract

The invention discloses an egg yolk oil with anti-allergic effect and a low-temperature extraction and purification process thereof. The egg yolk oil with anti-allergic effect is prepared by a supercritical carbon dioxide low-temperature extraction process using an egg yolk raw material under the action of an entrainer and a modifier. The invention can improve the oil yield of the egg yolk raw material under the supercritical carbon dioxide low-temperature extraction process by further improving the solubility and selectivity of the egg yolk raw material with the entrainer and the modifier, and can effectively extract the anti-allergic components in the egg yolk oil, so that the prepared egg yolk oil has anti-allergic effect, improves the application value of the egg yolk oil, avoids byproducts that may be generated due to high temperature, and further improves the safety of the egg yolk oil.

Description

Technical Field

[0001] The invention relates to the technical field of food and medicine, and in particular to egg yolk oil with anti-allergic effect and a low-temperature extraction and purification process thereof. Background Art

[0002] Egg yolk oil, also known as phoenix liquid, chicken oil, and egg yolk lipid, is an egg yolk extract obtained by separation and extraction of fresh poultry eggs. It is rich in nutrients and has high clinical application value. Egg yolk oil contains triglycerides (TG), cholesterol (CHO), phosphatidylcholine (Pc), cephalin (PE), protein, a small amount of water and trace riboflavin and other nutrients. It is widely used in clinical medicine, health food, cosmetics, medicine and chemical industries.

[0003] At present, the traditional methods for extracting egg yolk oil include organic solvent method, dry distillation method, enzyme method, supercritical CO2 extraction method, etc. Among them, the organic solvent method has small equipment investment, the required solvent is easy to obtain, and the production cost is low, but its shortcomings are: a. The process is cumbersome and takes a long time; b. The solvent recovery consumes a lot of energy, the loss is large, and it is easy to remain; c. The oil yield is low and the product purity is low; for example: using egg yolk powder as raw material, ethanol with a concentration of ≥98% (v) as the extractant, the extraction temperature is 60°C, and four extractions are used to absorb the supernatant. The oil yield of the small test is 60%, the oil yield of the pilot test is 57%, and the direct production cost is 86,007 yuan / t (oil). The dry distillation method is simple to prepare, but the oil yield is very low, the product color is dark, the components are decomposed and destroyed, the quality is poor, and mass production is prone to environmental pollution. The enzyme method extracts egg yolk oil from egg yolk powder with an yield of 58.89%.

[0004] Professor Liang Liguo of the School of Life Sciences at CUHK said that the oil in egg yolks may produce carcinogens at high temperatures, and long-term exposure will increase the risk of skin cancer. The first step in making homemade egg yolk oil is to boil the eggs; the second step is to dry-fry the cooked egg yolks. In fact, frying the egg yolks at high temperatures for a long time may have destroyed the lipids and vitamins in the egg yolks. The scorched egg yolks are because the lipid molecules undergo "polymerization" at high temperatures. In addition to producing lipid polymers, the oil in the egg yolks at high temperatures may also produce carcinogenic "polycyclic aromatic hydrocarbons". Long-term exposure will pose a risk of cancer.

[0005] Supercritical carbon dioxide extraction is a high-tech method with the advantages of simplifying the extraction steps, easy separation of the extractant, reduced solvent consumption, no solvent residue, reduced energy consumption, and good product quality. The egg yolk is extracted by supercritical carbon dioxide extraction at low temperature, with high purity and no impurities left after extraction. Low-temperature extraction does not destroy the nutrients in the egg yolk, and is rich in lecithin, saturated fatty acids, unsaturated fatty acids, vitamins AD, etc.

[0006] However, the oil yield of the egg yolk oil extraction process in the prior art is low, and the higher extraction process will lead to the destruction of its nutritional components, affecting the efficacy of the egg yolk oil.

[0007] Therefore, there is an urgent need for an extraction process that can be performed under low temperature conditions with a high oil yield and can make the prepared egg yolk oil have anti-allergic effects. Summary of the invention

[0008] Purpose of the invention: In view of the defects of the prior art, the purpose of the present invention is to provide a low-temperature extraction and purification process that can be used for extraction under low-temperature conditions with a high oil yield, and at the same time can make the prepared egg yolk oil have anti-allergic effects.

[0009] Technical solution:

[0010] The invention discloses a low-temperature extraction and purification process of egg yolk oil with anti-allergic effect. The egg yolk oil with anti-allergic effect is prepared by using egg yolk raw materials in the presence of an entrainer and a modifier through a supercritical carbon dioxide low-temperature extraction process.

[0011] The present invention can effectively extract the anti-allergic components in the egg yolk raw material by extracting the egg yolk raw material through a supercritical carbon dioxide low-temperature extraction process, and maintain the activity of the anti-allergic components at a relatively low temperature, thereby giving the egg yolk oil an anti-allergic effect and improving the application value of the egg yolk oil.

[0012] Furthermore, the low-temperature extraction and purification process of egg yolk oil with anti-allergic effect comprises the following steps:

[0013] (1) placing the egg yolk raw material in a vacuum drying oven, drying at 35-40° C. to constant weight, taking it out, crushing it and sieving it to a particle size of 40-60 meshes to obtain a crude raw material for later use;

[0014] (2) Add the crude raw material into the extraction kettle, add the entrainer and the modifier into the carrying agent tank and mix them evenly;

[0015] (3) The carbon dioxide is brought into a supercritical state by a booster pump and a preheater and introduced into the extraction kettle, and at the same time, the material in the carrier tank is uniformly flowed into the extraction kettle;

[0016] (4) pressurizing and heating the extraction kettle to perform extraction;

[0017] (5) After the extraction is completed, the supercritical carbon dioxide in the extraction kettle is cooled and slowly released to keep the pressure balanced with the outside, and after removing the entrainer, the extract is taken out to obtain the egg yolk oil with anti-allergic effect.

[0018] The present invention extracts the effective components in the egg yolk raw material through a supercritical carbon dioxide low-temperature extraction process. On the one hand, supercritical carbon dioxide has high solubility and selectivity for the effective components and anti-allergic components in the egg yolk powder, and can effectively extract the effective components and anti-allergic components in the egg yolk oil with high purity; on the other hand, the supercritical carbon dioxide extraction process can be carried out under relatively low temperature conditions, which can avoid the inactivation and denaturation of the effective components of the egg yolk oil under high temperature conditions, thereby avoiding the generation of by-products with carcinogenicity, and can further improve the safety of the egg yolk oil.

[0019] Furthermore, in step (1), the egg yolk raw material is selected from egg yolk powder or egg yolk.

[0020] Furthermore, the entrainer in step (2) is prepared by mixing ethanol and ethyl acetate in a mass ratio of 1:2-3.

[0021] The present invention can further improve the solubility and selectivity of egg yolk oil and anti-allergic components in supercritical carbon dioxide by adding an entrainer prepared by combining ethanol and ethyl acetate in a supercritical carbon dioxide low-temperature extraction process, so that they can be effectively extracted and purified, thereby enabling the low-temperature extraction and purification process to have a higher oil yield and higher product purity.

[0022] Furthermore, in the step (2), the modifier is prepared by mixing sodium alginate and betaine in a mass ratio of 1:3-5.

[0023] The present invention adds a modifier formed by a composite of sodium alginate and betaine in a supercritical carbon dioxide low-temperature extraction process. On the one hand, betaine has a certain synergistic function and can be effectively and evenly combined in the egg yolk oil structure by being introduced into an extraction kettle together with an entrainer, thereby further improving the anti-allergic effect of the egg yolk oil. On the other hand, sodium alginate can improve the viscosity and stability of the egg yolk oil, thereby effectively separating the egg yolk oil. Moreover, after the sodium alginate and betaine are composited, the compatibility of betaine in the egg yolk oil can be improved, thereby further improving the stability of the egg yolk oil.

[0024] Furthermore, in the step (2), the mass ratio of the entrainer to the modifier is (15-20): (4-6).

[0025] Furthermore, in the step (3), the mass ratio of the crude raw material to the material in the carrying agent tank is (50-60): (5-8).

[0026] Furthermore, in step (3), the flow rate of supercritical carbon dioxide is 20-30 L / h.

[0027] Furthermore, in step (4), the temperature of the extraction kettle is 32-35° C., the pressure of the extraction kettle is 40-50 MPa, and the extraction time is 4-8 hours.

[0028] The egg yolk oil with anti-allergic effect is prepared by any one of the above-mentioned egg yolk oil low-temperature extraction and purification processes with anti-allergic effect.

[0029] Beneficial effects:

[0030] (1) The egg yolk oil with anti-allergic effect and the low-temperature extraction and purification process thereof provided by the present invention can improve the oil yield of the egg yolk raw material under the supercritical carbon dioxide low-temperature extraction process by further improving the solubility and selectivity of the egg yolk raw material with the help of entrainers and modifiers, and can effectively extract the anti-allergic components in the egg yolk oil, so that the prepared egg yolk oil has anti-allergic effect, improves the application value of the egg yolk oil, avoids the by-products that may be produced due to high temperature, and further improves the safety of the egg yolk oil.

[0031] (2) The egg yolk oil with anti-allergic effect and its low-temperature extraction and purification process provided by the present invention can effectively extract the anti-allergic components in the egg yolk raw material by extracting the egg yolk raw material through a supercritical carbon dioxide low-temperature extraction process, and maintain the activity of the anti-allergic components at a relatively low temperature, thereby giving the egg yolk oil an anti-allergic effect and improving the application value of the egg yolk oil.

[0032] (3) The egg yolk oil with anti-allergic effect and its low-temperature extraction and purification process provided by the present invention extract the effective ingredients in the egg yolk raw material through a supercritical carbon dioxide low-temperature extraction process. On the one hand, supercritical carbon dioxide has high solubility and selectivity for the effective ingredients and anti-allergic components in egg yolk powder, and can effectively extract the effective ingredients and anti-allergic components in egg yolk oil with high purity; on the other hand, the supercritical carbon dioxide extraction process can be carried out under relatively low temperature conditions, which can avoid the inactivation and denaturation of the effective ingredients in the egg yolk oil under high temperature conditions, and further avoid the production of carcinogenic by-products, which can further improve the safety of egg yolk oil.

[0033] (4) The egg yolk oil with anti-allergic effect and its low-temperature extraction and purification process provided by the present invention can further improve the solubility and selectivity of the egg yolk oil and anti-allergic components in the supercritical carbon dioxide by adding an entrainer prepared by a composite of ethanol and ethyl acetate in the supercritical carbon dioxide low-temperature extraction process, so that it can be effectively extracted and purified, thereby making the low-temperature extraction and purification process have a higher oil yield and higher product purity.

[0034] (5) The egg yolk oil with anti-allergic effect and its low-temperature extraction and purification process provided by the present invention are characterized by adding a modifier composed of sodium alginate and betaine in the supercritical carbon dioxide low-temperature extraction process. On the one hand, betaine has a certain synergistic function. By passing it into the extraction kettle together with the entrainer, it can be effectively and evenly combined in the egg yolk oil structure, further improving the anti-allergic effect of the egg yolk oil; on the other hand, sodium alginate can improve the viscosity and stability of the egg yolk oil, so that it can be effectively separated, and the combination of sodium alginate and betaine can improve the compatibility of betaine in the egg yolk oil, further improving the stability of the egg yolk oil. DETAILED DESCRIPTION

[0035] The present invention will be described below in conjunction with specific embodiments. It should be noted that the following embodiments are examples of the present invention and are only used to illustrate the present invention, but not to limit the present invention. Other combinations and various modifications within the concept of the present invention may be performed without departing from the spirit or scope of the present invention.

[0036] The commercially available egg yolk oil is supercritical extraction egg yolk oil purchased from Wuhan Kemik Biopharmaceutical Technology Co., Ltd.; the remaining reagents and equipment are conventional reagents and equipment in the technical field.

[0037] Example 1

[0038] The egg yolk oil with anti-allergic effect is prepared by the following process: by weight,

[0039] (1) Place 100 parts of egg yolk powder in a vacuum drying oven, dry at 40° C. to constant weight, take out, crush and sieve to a particle size of 50 mesh, and obtain a crude raw material for later use;

[0040] (2) Add 50 parts of crude raw material into the extraction kettle, add 1.25 parts of ethanol, 3.75 parts of ethyl acetate, 0.3 parts of sodium alginate and 1.2 parts of betaine into the carrying agent tank and mix well;

[0041] (3) The carbon dioxide is brought into a supercritical state by a booster pump and a preheater and introduced into the extraction kettle at a flow rate of 25 L / h, while the material in the carrier tank is uniformly flowed into the extraction kettle;

[0042] (4) pressurizing the extraction kettle to 45 MPa, heating it to 33° C., and extracting for 6 hours;

[0043] (5) After the extraction is completed, the supercritical carbon dioxide in the extraction kettle is cooled and slowly released to keep the pressure balanced with the outside, and after removing the entrainer, the extract is taken out to obtain the egg yolk oil with anti-allergic effect.

[0044] Example 2

[0045] The method is basically the same as Example 1, except that the ingredients in the carrying agent tank in step (2) are changed to 1.6 parts of ethanol, 3.4 parts of ethyl acetate, 0.4 parts of sodium alginate and 1.2 parts of betaine.

[0046] Example 3

[0047] The method is basically the same as Example 1, except that the ingredients in the carrying agent tank in step (2) are changed to 1.25 parts of ethanol, 3.75 parts of ethyl acetate, 0.4 parts of sodium alginate and 1.2 parts of betaine.

[0048] Comparative Example 1

[0049] Commercially available egg yolk oil.

[0050] Comparative Example 2

[0051] Take 1000g of egg yolk powder and extract the egg yolk oil by supercritical carbon dioxide extraction. The extraction temperature is 50°C, the extraction pressure is 38Mpa, the CO2 flow rate is 40L / h, and the extraction time is 6 hours.

[0052] Comparative Example 3

[0053] The method is basically the same as Example 1, except that no carrying agent tank is provided in step (2) and step (3).

[0054] Comparative Example 4

[0055] The method is basically the same as Example 1, except that in step (2), 0.3 parts of sodium alginate and 1.2 parts of betaine are replaced by 1.5 parts of ethanol.

[0056] Comparative Example 5

[0057] The method is basically the same as Example 1, except that in step (2), 1.25 parts of ethanol and 3.75 parts of ethyl acetate are replaced by 5 parts of ethanol.

[0058] Performance Testing

[0059] Oil yield detection: The quality of the products obtained after the process of Examples 1-3 and Comparative Examples 2-5 was detected, and the oil yield was calculated according to the principle of oil yield = product quality / raw material quality × 100%.

[0060] Anti-allergic ability test: The anti-allergic ability of the products obtained after the process of Examples 1-3 and Comparative Examples 1-5 was tested by hyaluronidase activity inhibition test. The specific test method is as follows:

[0061] Detection principle: When allergens invade the body for the first time, the body produces antibody IgE. When allergens invade the body again, they combine with IgE antibodies on the surface of sensitized cells, causing FceRI cross-linking, thereby starting activation signals, triggering signal transduction, and activating multiple enzymes including intracellular hyaluronidase. This process is called an allergic reaction. Hyaluronic acid is a component in the tissue matrix that limits the diffusion of water and other extracellular substances. After being hydrolyzed by hyaluronidase, the cells become non-viscous, causing cell degranulation and exudation of new synthesized media, exerting biological effects, and leading to the occurrence of immediate allergic reactions. Hyaluronidase is a participant in allergic reactions. Studies have shown that hyaluronidase is closely related to inflammation and allergies. Inhibiting the activity of hyaluronidase can prevent hyaluronic acid from being decomposed, maintain normal physiological functions, and thus achieve anti-allergic effects. The higher the inhibition rate of hyaluronidase activity, the stronger the anti-allergic effect of the substance, and vice versa. Therefore, the inhibition of hyaluronidase activity can be used as an indicator of anti-inflammatory and anti-allergic reactions of samples.

[0062] Detection steps: Take 0.1mL 0.25mmol / L calcium chloride aqueous solution and 0.5mL hyaluronidase solution, mix them evenly, and keep them at 37°C for 20min; add 0.5mL of the products of Examples 1-3 and Comparative Examples 1-5 respectively, and keep them at 37°C for 20min; add 0.5mL sodium hyaluronate solution, keep it at 37°C for 30min, and place it at room temperature for 5min; add 0.1mL 0.4mol / L NaOH aqueous solution and 0.5mL acetylacetone solution, place it in a boiling water bath and heat it for 15min, then immediately cool it on ice for 5min; add 1.0mL Ehrlich reagent, dilute it with 3.0mL anhydrous ethanol, and place it for 20min to develop color; measure the absorbance value at 547nm with a spectrophotometer, and substitute it into the following formula to calculate the inhibition rate:

[0063] Hyaluronic acid inhibition rate = [(AB)-(CD)] / (AB)*100%

[0064] Where: A is the absorbance of the control solution (using acetate buffer instead of sample solution);

[0065] B is the absorbance of the control blank solution (using acetate buffer instead of sample solution and enzyme solution);

[0066] C is the absorbance of the sample solution;

[0067] D is the absorbance of the blank solution of the sample (using acetate buffer instead of enzyme solution).

[0068] The test results are shown in the following table:

[0069]

[0070] According to the comparison of the test results of Examples 1-3 and Comparative Examples 1-2, the egg yolk oil with anti-allergic effect and its low-temperature extraction and purification process provided by the present invention can give the egg yolk oil anti-allergic effect and can improve the oil yield of the supercritical carbon dioxide extraction process.

[0071] According to the comparison of the test results of Examples 1-3 and Comparative Examples 3-5, it can be seen that in the egg yolk oil with anti-allergic efficacy and its low-temperature extraction and purification process provided by the present invention, by adding entrainers and modifiers, the solubility and selectivity of the effective ingredients and anti-allergic components in the egg yolk oil in supercritical carbon dioxide can be improved, the oil yield can be improved, and the anti-allergic efficacy of the egg yolk oil can be further improved.

[0072] The above implementation modes are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with this technology to understand the content of the present invention and implement it, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A low-temperature extraction and purification process for egg yolk oil with anti-allergic effect, characterized in that: The egg yolk oil with anti-allergic effect is prepared by using egg yolk raw materials in the presence of an entrainer and a modifier, and then subjected to a supercritical carbon dioxide low-temperature extraction process; The low-temperature extraction and purification process of egg yolk oil with anti-allergic effect comprises the following steps: (1) Place the egg yolk raw material in a vacuum drying oven and dry it at 35-40°C until constant weight is reached. After taking it out, crush it and sieve it to a particle size of 40-60 mesh to obtain a crude raw material for later use; (2) Add the crude raw material into the extraction kettle, add the entrainer and modifier into the carrying agent tank and mix them evenly; (3) The carbon dioxide is brought into a supercritical state through a booster pump and a preheater and introduced into the extraction kettle, while the material in the carrier tank is uniformly flowed into the extraction kettle; (4) Pressurizing and heating the extraction kettle to perform extraction; (5) After the extraction is completed, the supercritical carbon dioxide in the extraction kettle is cooled and slowly released to keep the pressure balanced with the outside, and after removing the entrainer, the extract is taken out to obtain the egg yolk oil with anti-allergic effect; In step (2), the entrainer is prepared by mixing ethanol and ethyl acetate in a mass ratio of 1:2-3; In step (2), the modifier is prepared by mixing sodium alginate and betaine in a mass ratio of 1:3-5; The mass ratio of the entrainer to the modifier in the step (2) is (15-20):(4-6).

2. The low-temperature extraction and purification process of egg yolk oil with anti-allergic effect according to claim 1, characterized in that: In the step (1), the egg yolk raw material is selected from egg yolk powder or egg yolk.

3. The low-temperature extraction and purification process of egg yolk oil with anti-allergic effect according to claim 1, characterized in that: In the step (3), the mass ratio of the crude raw material to the material in the carrying agent tank is (50-60): (5-8).

4. The low-temperature extraction and purification process of egg yolk oil with anti-allergic effect according to claim 1, characterized in that: The flow rate of supercritical carbon dioxide in step (3) is 20-30 L / h.

5. The low-temperature extraction and purification process of egg yolk oil with anti-allergic effect according to claim 1, characterized in that: In the step (4), the temperature of the extraction kettle is 32-35° C., the pressure of the extraction kettle is 40-50 MPa, and the extraction time is 4-8 hours.

6. Egg yolk oil with anti-allergic effect obtained by the low-temperature extraction and purification process of egg yolk oil with anti-allergic effect as described in any one of claims 1 to 5.

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