Longan pulp polyphenol extract as well as extraction method and application thereof
Patent Information
- Application Number
- CN202510333514.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-20
- Publication Date
- 2025-05-13
- Estimated Expiration
- Not applicable · inactive patent
Abstract
Description
Technical Field
[0001] The present application relates to the field of biological extraction technology, and in particular to a longan pulp polyphenol extract and an extraction method and application thereof. Background Art
[0002] Longan flesh is rich in a variety of nutrients, among which polyphenols have multiple biological activities such as antioxidant, anti-inflammatory and anti-cancer, and have broad application prospects in the fields of food, medicine and cosmetics. At present, the traditional methods for extracting polyphenols from longan flesh mainly include solvent extraction, ultrasonic-assisted extraction and microwave-assisted extraction. Solvent extraction has problems such as low extraction rate and residual organic solvent; although ultrasonic-assisted extraction and microwave-assisted extraction can improve the extraction efficiency to a certain extent, they still have disadvantages such as high energy consumption and complex equipment requirements. With the continuous development of science and technology, some new extraction technologies have gradually emerged, such as supercritical fluid extraction technology and enzymatic hydrolysis, which provide new ideas for the extraction of polyphenols from longan flesh. Therefore, it is of great practical significance to develop an efficient, environmentally friendly, novel and creative method for extracting polyphenols from longan flesh. Summary of the invention
[0003] In view of this, the present application provides a longan pulp polyphenol extract and an extraction method and application thereof. The extraction method has the advantages of high extraction rate, low energy consumption, environmental protection and pollution-free, simple operation, etc., and can effectively overcome the defects of the above-mentioned prior art.
[0004] The first aspect of the present application provides a method for extracting polyphenols from longan pulp, comprising the following steps:
[0005] S1, subjecting the pretreated longan pulp powder to supercritical carbon dioxide extraction, whereby polyphenols in the longan pulp are extracted into the carbon dioxide phase under supercritical conditions;
[0006] S2, the residue after supercritical carbon dioxide extraction is taken out, an appropriate amount of deionized water is added to prepare a longan pulp suspension, an enzyme preparation is added to the longan pulp suspension for enzymolysis-assisted extraction, and the enzymolysis solution is centrifuged after the enzymolysis is completed, and the supernatant is collected;
[0007] S3. Concentrating and purifying the supernatant, and freeze-drying to obtain a high-purity longan pulp polyphenol extract.
[0008] Preferably, in step S1, the specific process of the supercritical carbon dioxide extraction is: placing the pretreated longan pulp powder into an extraction kettle of a supercritical carbon dioxide extraction device for supercritical carbon dioxide extraction, using carbon dioxide as the extraction agent, and the entrainer as an ethanol aqueous solution with a volume fraction of 50%, and the mass ratio of the entrainer to the pretreated longan pulp powder is 1:5; setting the extraction pressure to 30-32MPa, the extraction temperature to 45-48°C, the extraction time to 2-2.5h, and the carbon dioxide flow rate to 20-25L / h.
[0009] Preferably, in step S1, the pretreatment process of the longan flesh is: select fresh, disease- and insect-free longan fruits, remove the core and take out the flesh, wash the longan flesh and cut it into small pieces, put it into a freeze dryer for freeze drying, freeze dry it at -50 to -55°C for 20-24h to obtain a dried longan flesh sample, crush the dried longan flesh sample, pass it through a 40-mesh sieve, obtain the pretreated longan flesh powder, and set it aside.
[0010] Preferably, in step S2, the specific process of the enzymatic hydrolysis-assisted extraction is: adding a composite enzyme preparation of cellulase and pectinase to the longan pulp suspension, adjusting the pH value of the suspension to 5.0, and performing enzymolysis in a constant temperature water bath at 50-52°C for 3-3.5 hours with continuous stirring during the process.
[0011] Preferably, the mass ratio of the cellulase to the pectinase is 2:1, and the added amount of the complex enzyme preparation is 0.5% of the mass of the longan pulp suspension.
[0012] Preferably, in step S2, the mass fraction of the longan pulp suspension is 10%.
[0013] Preferably, in step S3, the specific process of concentration and purification is: the supernatant is concentrated under reduced pressure using a rotary evaporator to remove most of the water to obtain a concentrated solution; the concentrated solution is purified by a macroporous adsorption resin column, the resin column is first rinsed with deionized water to remove impurities, and then the polyphenols are eluted with an ethanol solution with a volume fraction of 70%, and the eluate is collected; the eluate is again concentrated under reduced pressure.
[0014] Preferably, in step S3, the specific conditions of freeze drying are: freeze drying in a freeze dryer at -50 to -55°C for 20 to 24 hours.
[0015] The second aspect of the present application also provides a longan pulp polyphenol extract, which is prepared by the above-mentioned method.
[0016] The third aspect of the present application also provides the application of the longan pulp polyphenol extract in the fields of food, medicine and cosmetics.
[0017] Compared with the prior art, this application has the following beneficial effects:
[0018] 1. High extraction rate: This application combines supercritical carbon dioxide extraction with enzymatic assisted extraction, giving full play to the advantages of the two technologies, and can more effectively extract polyphenols from longan flesh. Compared with traditional methods, the extraction rate is increased by more than 30%.
[0019] 2. Low energy consumption: The supercritical carbon dioxide extraction of the present application is carried out under relatively mild conditions, which reduces energy consumption; the enzymatic hydrolysis reaction can be carried out at 50°C, which further reduces energy consumption.
[0020] 3. Environmentally friendly and pollution-free: The supercritical carbon dioxide extraction in this application uses carbon dioxide as the extraction agent. Carbon dioxide is non-toxic, odorless, pollution-free, and recyclable; the enzyme preparation used in the enzymatic hydrolysis process is a biocatalyst and is environmentally friendly.
[0021] 4. Simple operation: The process flow of the method for extracting polyphenols from longan pulp in the present application is relatively simple, the equipment requirements are not high, and it is easy to industrialize production. DETAILED DESCRIPTION
[0022] In order to make the purpose, technical solution and advantages of this application clearer, the technical solution in this application will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.
[0023] Unless otherwise specified, the experimental methods used in the examples of this application are all conventional methods.
[0024] In the following examples, unless otherwise specified, all raw materials can be obtained by commercial purchase or conventional methods.
[0025] Example 1
[0026] Raw material pretreatment: 10 kg of fresh, pest-free longan fruits were selected, the cores were removed, the flesh was washed and cut into small pieces, and placed in a freeze dryer, freeze-dried at -50°C for 24 hours to obtain 2.5 kg of dried longan flesh. The dried longan flesh was crushed and passed through a 40-mesh sieve to obtain 2.3 kg of pretreated longan flesh powder.
[0027] Supercritical carbon dioxide extraction: put 2kg of pretreated longan pulp powder into the extraction kettle of supercritical carbon dioxide extraction device, use carbon dioxide as extraction agent, entrainer as 50% ethanol aqueous solution, and the mass ratio of entrainer to pretreated longan pulp powder is 1:5. Set the extraction pressure to 30MPa, the extraction temperature to 45℃, the extraction time to 2h, and the carbon dioxide flow rate to 20L / h. After the extraction, collect the extract.
[0028] Enzyme-assisted extraction: Take out the residue after supercritical carbon dioxide extraction, add 10L of deionized water, and prepare a 10% longan pulp suspension. Add 100g of a composite enzyme preparation of cellulase and pectinase (the mass ratio of cellulase to pectinase is 2:1) to the suspension, adjust the pH value of the suspension to 5.0, and perform enzymolysis in a constant temperature water bath at 50°C for 3h, stirring continuously. After the enzymolysis is completed, centrifuge the enzymolysis solution at a speed of 4000r / min for 15min, and collect the supernatant.
[0029] Concentration and purification: The supernatant was concentrated to a volume of 1L by a rotary evaporator at 60°C and 0.08MPa to obtain a concentrated solution. The concentrated solution was purified by a macroporous adsorption resin column (D101 type, column volume of 2L), and the resin column was first rinsed with 5L of deionized water to remove impurities, and then the polyphenols were eluted with 3L of 70% ethanol solution by volume, and the eluate was collected. The eluate was again concentrated to dryness under reduced pressure at 60°C and 0.08MPa, and then placed in a freeze dryer and freeze-dried at -50°C for 24h to obtain 120g of longan pulp polyphenol extract. After testing, the content of polyphenols in the extract was 95%.
[0030] Example 2
[0031] Raw material pretreatment: 15 kg of fresh, pest-free longan fruits were selected, the cores were removed, the flesh was washed and cut into small pieces, and placed in a freeze dryer, freeze-dried at -55°C for 20 hours to obtain 3.8 kg of dried longan flesh. The dried longan flesh was crushed and passed through a 40-mesh sieve to obtain 3.5 kg of pretreated longan flesh powder.
[0032] Supercritical carbon dioxide extraction: 3kg of pretreated longan pulp powder was placed in the extraction kettle of the supercritical carbon dioxide extraction device, with carbon dioxide as the extractant, the entrainer as a 50% ethanol aqueous solution, and the mass ratio of the entrainer to the pretreated longan pulp powder was 1:5. The extraction pressure was set to 32MPa, the extraction temperature was 48°C, the extraction time was 2.5h, and the carbon dioxide flow rate was 25L / h. After the extraction was completed, the extract was collected.
[0033] Enzyme-assisted extraction: Take out the residue after supercritical carbon dioxide extraction, add 15L of deionized water, and prepare a longan pulp suspension with a mass fraction of 10%. Add 150g of a composite enzyme preparation of cellulase and pectinase (the mass ratio of cellulase to pectinase is 2:1) to the suspension, adjust the pH value of the suspension to 5.0, and perform enzymolysis in a constant temperature water bath at 52°C for 3.5h, stirring continuously during the period. After the enzymolysis is completed, the enzymolysis solution is centrifuged at a speed of 4500r / min for 15min, and the supernatant is collected.
[0034] Concentration and purification: The supernatant was concentrated to a volume of 1.5 L by a rotary evaporator at 65°C and 0.09 MPa to obtain a concentrated solution. The concentrated solution was purified by a macroporous adsorption resin column (AB-8 type, column volume of 3 L), and the resin column was first rinsed with 7 L of deionized water to remove impurities, and then the polyphenols were eluted with 4 L of 70% ethanol solution by volume, and the eluate was collected. The eluate was again concentrated to dryness under reduced pressure at 65°C and 0.09 MPa, and then placed in a freeze dryer and freeze-dried at -55°C for 20 hours to obtain 180 g of longan pulp polyphenol extract. After testing, the content of polyphenols in the extract was 96%.
[0035] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.
Claims
1. A method for extracting polyphenols from longan pulp, characterized in that: The following steps are involved: S1, subjecting the pretreated longan pulp powder to supercritical carbon dioxide extraction, where the polyphenols in the longan pulp are extracted into the carbon dioxide phase under supercritical conditions; S2, the residue after supercritical carbon dioxide extraction is taken out, an appropriate amount of deionized water is added to prepare a longan pulp suspension, an enzyme preparation is added to the longan pulp suspension for enzymolysis-assisted extraction, and the enzymolysis solution is centrifuged after the enzymolysis is completed, and the supernatant is collected; S3. Concentrating and purifying the supernatant, and freeze-drying to obtain a high-purity longan pulp polyphenol extract.
2. The method for extracting polyphenols from longan pulp according to claim 1, characterized in that: In step S1, the specific process of the supercritical carbon dioxide extraction is: putting the pretreated longan pulp powder into the extraction kettle of the supercritical carbon dioxide extraction device for supercritical carbon dioxide extraction, using carbon dioxide as the extraction agent, the entrainer as an ethanol aqueous solution with a volume fraction of 50%, and the mass ratio of the entrainer to the pretreated longan pulp powder is 1:5; setting the extraction pressure to 30-32MPa, the extraction temperature to 45-48°C, the extraction time to 2-2.5h, and the carbon dioxide flow rate to 20-25L / h.
3. The method for extracting polyphenols from longan pulp according to claim 1, characterized in that: In step S1, the pretreatment process of the longan flesh is as follows: fresh longan fruits free of disease and insect pests are selected, the cores are removed and the flesh is taken out, the longan flesh is washed and cut into small pieces, and the pieces are put into a freeze dryer for freeze drying, and freeze dried at -50 to -55°C for 20-24h to obtain a dried longan flesh sample, and the dried longan flesh sample is crushed and passed through a 40-mesh sieve to obtain pretreated longan flesh powder for later use.
4. The method for extracting polyphenols from longan pulp according to claim 1, characterized in that: In step S2, the specific process of the enzymatic hydrolysis-assisted extraction is: adding a composite enzyme preparation of cellulase and pectinase to the longan pulp suspension, adjusting the pH value of the suspension to 5.0, and performing enzymolysis in a constant temperature water bath at 50-52° C. for 3-3.5 hours with continuous stirring during the process.
5. The method for extracting polyphenols from longan pulp according to claim 4, characterized in that: The mass ratio of the cellulase to the pectinase is 2:1, and the added amount of the composite enzyme preparation is 0.5% of the mass of the longan pulp suspension.
6. The method for extracting polyphenols from longan pulp according to claim 1, characterized in that: In step S2, the mass fraction of the longan pulp suspension is 10%.
7. The method for extracting polyphenols from longan pulp according to claim 1, characterized in that: In step S3, the specific process of concentration and purification is: the supernatant is concentrated under reduced pressure using a rotary evaporator to remove most of the water to obtain a concentrated solution; the concentrated solution is purified by a macroporous adsorption resin column, the resin column is first rinsed with deionized water to remove impurities, and then the polyphenols are eluted with an ethanol solution with a volume fraction of 70%, and the eluate is collected; the eluate is again concentrated under reduced pressure.
8. The method for extracting polyphenols from longan pulp according to claim 1, characterized in that: In step S3, the specific conditions of freeze drying are: freeze drying in a freeze dryer at -50 to -55°C for 20 to 24 hours.
9. A longan pulp polyphenol extract, characterized in that: A longan pulp polyphenol extract prepared by the method described in any one of claims 1 to 8.
10. Use of the longan pulp polyphenol extract according to claim 9 in the fields of food, medicine and cosmetics.