Water extraction process of propolis supercritical raffinate as well as product and application thereof

Abstract

The invention belongs to the technical field of propolis extraction, and particularly relates to a water extraction process of propolis supercritical raffinate as well as a product and application of the propolis supercritical raffinate. In the propolis extraction technology, the extraction residue is researched, the polar solvent characteristic of water is ingeniously utilized, the supercritical CO2 extraction residue is subjected to secondary extraction, and ultrahigh pressure and catalytic infrared radiation treatment are combined, so that the extraction process which is more efficient, quicker, safer and more economical is provided. In addition, water is used as a solvent in the preparation process of the propolis extract, so that non-polar residues, possibly from the nature or human intervention, in the structure of raw propolis can be prevented from entering the final extract; the obtained final extract is safe and free of peculiar smell, has good antibacterial activity and can be well used for preparing oral care products. The method not only realizes full utilization of the raffinate after propolis processing, but also obtains an effective scheme, and has a good market application prospect.

Description

Technical Field

[0001] The invention belongs to the technical field of propolis extraction, and in particular relates to a water extraction process of propolis supercritical extract residue and a product and application thereof. Background Art

[0002] Propolis is a resinous substance collected by worker bees from the apical buds and exudates of plants, mixed with beeswax and the secretions of the bees' maxillary glands, and processed into a sticky solid with an aromatic smell. Propolis has a wide range of biological and pharmacological activities. For example, propolis is rich in flavonoids and phenolic acids, which make it have multiple functions such as antibacterial, antioxidant, immune-enhancing, blood sugar-lowering, and blood lipid-lowering, and has a very good health-care effect on the human body.

[0003] As a traditional Chinese medicine, propolis cannot be produced and sold as a common food raw material, that is, it cannot be used in the food industry in its original form, so propolis needs to be used in a targeted and reasonable manner. Propolis extraction is generally a necessary process for the use of propolis. At present, the mainstream propolis extraction methods are mainly solvent extraction and supercritical carbon dioxide (CO 2 ) extraction technology. Among the solvent extraction methods, ethanol is the most commonly used solvent for extracting propolis due to its large dipole moment. Supercritical CO 2 The extraction technology utilizes the dual properties of carbon dioxide in the supercritical state, which is both gas and liquid. In this way, substances can be dissolved from the matrix; then, by reducing the pressure of the carrier gas or increasing the temperature, the supercritical CO 2 The solubility will decrease, thus achieving the goal of extraction and separation.

[0004] On the other hand, the research on propolis mainly focuses on how to use solvents or supercritical CO more efficiently. 2 Propolis is extracted by extraction technology, but there is a lack of targeted research on the residue after propolis extraction. These residues are usually regarded as waste residues and discarded, and their potential natural resource value cannot be fully utilized. Therefore, it is crucial to establish an effective method to realize the utilization of the residue after propolis extraction.

[0005] Ultrahigh pressure technology is a non-thermal processing high-tech technology that has attracted worldwide attention and extensive research. It refers to placing the material to be processed in a pressure system with water or other liquids as the pressure transmission medium and processing it under static liquid pressure. At the same time, it is widely used in the food industry because it has little effect on food components and can well maintain the color, aroma, taste, nutrition and functional components of food. It is a hot technical research topic at present.

[0006] Catalytic infrared heating is a technology that uses a catalyst to convert fuel gas into infrared radiation. It uses air as a heat transfer medium and controls the combination of combustible gas and oxygen on the surface of the catalyst layer to produce an oxidation reaction to generate medium and long-wave infrared radiation. The infrared radiation energy wavelength is within the far-infrared wavelength range and propagates in a straight line at the speed of light to reach the surface of the dried object. It is completely flameless and does not produce harmful gases or noise. It has the advantages of fast heating speed, controllable temperature, and high energy utilization rate. It is a low-carbon, clean, and energy-saving heating technology that has received widespread attention internationally.

[0007] At present, ultra-high pressure and catalytic infrared heating have received widespread attention as cutting-edge technologies. However, research on catalytic infrared heating is mainly concentrated in the field of drying, and research on ultra-high pressure technology is mainly concentrated in the fields of sterilization and food processing. There are few reports on its application in propolis extraction, which urgently needs further research. Summary of the invention

[0008] In view of the deficiencies of the prior art and to solve the above problems, the present invention provides a water extraction process for supercritical propolis residue, its products and uses; in the propolis extraction technology, the present invention studies the residue, directly uses water as the extraction solvent of the residue, combines ultra-high pressure and catalytic infrared radiation treatment, thereby providing a more efficient, faster, safer and more economical extraction process. In addition, the present invention uses water as a solvent in the preparation process of propolis extract, which can prevent non-polar residues in the structure of raw propolis that may come from nature or human intervention from entering the final extract; the obtained propolis water extract is safe and odorless, and has good antibacterial properties, and can be used for the preparation of oral care products. Not only has the full utilization of the residue after propolis processing been achieved, but also an effective solution has been achieved, with good market application prospects.

[0009] In order to achieve the above technical objectives, the technical solution provided by the present invention is as follows:

[0010] A water extraction process for propolis supercritical extract residue comprises the following steps:

[0011] (1) Using propolis propolis as a raw material, first freezing the propolis, then crushing it, and then sieving it to obtain propolis particles;

[0012] (2) Add the wool rubber particles obtained in step (1) into an extraction kettle, using carbon dioxide as the fluid, CO 2 The flow rate is 6-8L / min; the extraction pressure is adjusted to 25-30Mpa, the temperature is 30-50℃, and the time is 30-60min. Supercritical carbon dioxide extraction is performed and the CO is vented after extraction. 2 , complete the extraction and collect the residue after extraction, record it as the residue, and set it aside;

[0013] (3) adding the raffinate obtained in step (2) into water, stirring evenly and then subjecting to ultra-high pressure treatment, the pressure is 250-350 MPa, the temperature is 30° C.-40° C., the pressure holding time is 5-8 min, and the pressure is repeatedly increased and released several times to obtain an ultra-high pressure treated liquid;

[0014] (4) subjecting the ultrahigh pressure treated liquid obtained in step (3) to catalytic infrared radiation treatment, filtering and collecting the filtrate after the catalytic infrared radiation treatment, and finally subjecting the filtrate to low temperature concentration treatment to obtain a propolis water extract.

[0015] Preferably, the freezing treatment temperature in step (1) is -20°C to -5°C for 8-12 hours; and the mesh size of the sieve after crushing is 5-10 meshes.

[0016] Preferably, the extraction temperature in step (2) is 35-40°C.

[0017] Preferably, in step (3), the ratio of the amount of raffinate to the amount of water is 1 g: 2-10 mL.

[0018] Preferably, in step (3), the pressure increase and pressure relief in step 2 are repeated 2 to 3 times.

[0019] Preferably, the radiation temperature in step (4) is 65 to 85° C., the radiation distance is 25 to 40 cm, and the action time is 2 to 10 min.

[0020] The water extract prepared based on the above steps is used for antibacterial purposes.

[0021] An oral care product, the ingredients of which include propolis aqueous extract;

[0022] An oral care product comprises a mouthwash and an oral spray.

[0023] The cavity care product is propolis mouthwash, and the components are as follows:

[0024] Sorbitol 8-10%, glycerin 4-6%, propolis aqueous extract 2-10%, patchouli honey 1-6%, poloxamer 4071-2%, xylitol 1-2%, hydrogenated castor oil 0.2-0.4%, soybean polypeptide 1-2%, menthyl lactate 0.03-0.05%, honeysuckle extract 1-2%, licorice extract 1-2%, essence 0.03-0.05%, potassium sorbate 0.3-0.5%, deionized water balance.

[0025] The cavity care product is a propolis antibacterial oral spray, and the components are as follows:

[0026] Propolis water extract 8-15%, Patchouli honey 4-10%, honeysuckle extract 3-5%, monk fruit extract 2-4%, peppermint extract 2-4%, and deionized water as the balance.

[0027] The beneficial effects of the present invention are:

[0028] (1) Supercritical CO 2 Extraction technology can extract fat-soluble and non-polar substances in propolis; however, due to CO 2 The polarity is weak, and the extraction effect of the effective components with relatively large polarity is not good. It is not suitable to use supercritical CO for secondary extraction of the residue. 2 Extraction technology cannot effectively exert its effect. In the field of propolis solvent extraction, ethanol is a commonly used solvent, and extraction using ethanol is also a simple and efficient method. However, since ethanol is a polar solvent, it cannot extract most non-polar active ingredients, which leads to a certain degree of resource waste; in addition, the extract obtained by ethanol extraction is non-water-soluble, and an emulsifier needs to be added when applied to non-alcoholic solvents. However, the use of emulsifiers will change the natural properties of propolis and affect its antibacterial effect. Therefore, the application of propolis ethanol extract in oral care, cosmetics and other fields is subject to certain restrictions. Water, as a natural and healthy solvent, can also be used in the extraction field, but using only water as a solvent to extract propolis has a low utilization rate and poor economic benefits, resulting in a relatively slow industrialization process.

[0029] The present invention cleverly utilizes the polar solvent properties of water to treat supercritical CO 2 The residue is subjected to secondary extraction; the extraction efficiency of water-water solvent is significantly improved by creatively combining ultrahigh pressure and catalytic infrared radiation technology. The experimental results show that the extracted substances exhibit excellent antibacterial properties; while realizing the recycling of waste, the present invention also brings unexpected technical benefits.

[0030] (2) The present invention introduces ultra-high pressure treatment during the water extraction process. The ultra-high pressure can accelerate the diffusion rate of the infiltrating solute, allowing the aqueous solution to quickly infiltrate the residual material, and the medium can be changed to a high osmotic pressure state in a short time. After the pressure is released, the medium pressure can be quickly reduced. After repeated pressure increase and pressure release, the effective ingredients and the extract are fully in contact, which promotes the dissolution of polar components and achieves the dissolution of the effective ingredients in a short time. At the same time, the ultra-high pressure treatment can avoid the structural changes of the effective ingredients and the reduction of physiological activity caused by thermal effects, maintain the stability and activity of the ingredients, and not only has high extraction efficiency but also has the characteristics of less time consumption and low energy consumption.

[0031] (3) After ultra-high pressure treatment, the present invention further combines the use of catalytic infrared radiation for short-term treatment. Catalytic infrared can make the water in the material directly absorb infrared radiation energy and propagate in a straight line at the speed of light to reach the surface of the treatment liquid, thereby realizing rapid heating of the material. By utilizing the penetrating power of infrared radiation, the functional factors can be better diffused into the extraction solvent under the action of heat, which can not only further accelerate the dissolution of the effective ingredients, but also effectively ensure the stability of the dissolved material and will not affect the product quality. At the same time, it has the advantage of short time consumption, and the treatment can be completed within a few minutes, effectively reducing production costs and labor consumption. Finally, cryogenic concentration is used to obtain the extract. The principle of cryogenic concentration is to treat the liquid at low temperature to condense water molecules into solid ice, and then separate the solid ice to obtain concentrated substances. Cryogenic concentration has the advantage of low energy consumption and has broad industrial application prospects.

[0032] (4) The present invention uses water as the extraction solvent of the residue, and creatively combines ultrahigh pressure and catalytic infrared radiation treatment to solve the problem of low efficiency of using water alone as the extraction solvent, thereby providing a more efficient, faster, safer and more economical extraction process, and achieving unexpected technical effects. In addition, the present invention uses water as a solvent in the preparation process of propolis extract, which can also prevent non-polar residues in the structure of raw propolis that may come from nature or human intervention from entering the final extract; the obtained propolis water extract is safe and odorless, and has good antibacterial properties, and can be used in the preparation of oral care products. At the same time, due to its good antibacterial properties, it can be stored without pasteurization, sterilization or the addition of preservative additives. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a picture of the propolis aqueous extract prepared in Example 1.

[0034] Figure 2 The chromatogram is a chromatogram of the volatile components detected by GC-MS on the propolis water extract of Example 1. DETAILED DESCRIPTION

[0035] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0036] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0037] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.

[0038] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention without departing from the scope or spirit of the present invention. Other embodiments obtained from the present invention description will be apparent to those skilled in the art.

[0039] The method for obtaining the plant extract is as follows: honeysuckle, licorice, honeysuckle, mint and monk fruit are selected respectively, washed with clean water to remove impurities, dried and then crushed and sieved with a mesh size of 60 to 100 to obtain honeysuckle powder, licorice powder, honeysuckle powder, mint powder and monk fruit powder respectively; then the powders are added with 4 to 8 times the mass of pure water respectively, boiled for 5 to 10 minutes, maintained at 85 to 95° C. for continuous extraction for 60 to 90 minutes, the extract is centrifuged, filtered and impurity-removed by a centrifuge, and then concentrated at low temperature and vacuum to obtain honeysuckle extract, licorice extract, honeysuckle extract, mint extract and monk fruit extract.

[0040] Embodiment 1:

[0041] (1) Using propolis propolis as raw material, first freezing it at -20°C for 12 hours; then crushing it, and then passing it through a 5-mesh sieve to obtain propolis particles;

[0042] (2) Add the material obtained in step (1) into an extraction kettle, using carbon dioxide as the fluid, CO 2 The flow rate was 6L / min; the extraction pressure was adjusted to 30Mpa, the temperature was 35°C, and the time was 30min. Supercritical carbon dioxide extraction was performed and the CO was vented after extraction. 2 , complete the extraction and collect the residue after extraction, record it as the residue, and set it aside;

[0043] (3) adding the raffinate obtained in step (2) into water, wherein the ratio of the raffinate to the water is 1 g:4 mL; stirring evenly, performing ultrahigh pressure treatment, wherein the pressure is 300 MPa, the temperature is 40° C., the pressure holding time is 5 min, and the pressure is repeatedly increased and released 3 times to obtain an ultrahigh pressure treatment liquid;

[0044] (4) subjecting the ultrahigh pressure treatment liquid obtained in step (3) to catalytic infrared radiation treatment, wherein the radiation temperature is 65° C., the radiation distance is 30 cm, and the action time is 5 min; after the catalytic infrared radiation treatment, the filtrate is filtered and collected, and finally subjected to low temperature concentration treatment to obtain a propolis water extract.

[0045] Embodiment 2:

[0046] (1) Using propolis propolis as raw material, first freezing it at -20°C for 12 hours; then crushing it, and then passing it through a 5-mesh sieve to obtain propolis particles;

[0047] (2) Add the material obtained in step (1) into an extraction kettle, using carbon dioxide as the fluid, CO 2 The flow rate was 6L / min; the extraction pressure was adjusted to 25Mpa, the temperature was 35℃, and the time was 40min. Supercritical carbon dioxide extraction was performed and the CO was vented after extraction. 2 , complete the extraction and collect the residue after extraction, record it as the residue, and set it aside;

[0048] (3) adding the raffinate obtained in step (2) into water, wherein the ratio of the raffinate to the water is 1 g:4 mL; stirring evenly, performing ultrahigh pressure treatment, wherein the pressure is 250 MPa, the temperature is 40° C., the pressure holding time is 5 min, and the pressure is repeatedly increased and released twice to obtain an ultrahigh pressure treatment liquid;

[0049] (4) subjecting the ultrahigh pressure treated liquid obtained in step (3) to catalytic infrared radiation treatment, wherein the radiation temperature is 80° C., the radiation distance is 40 cm, and the action time is 4 min; after the catalytic infrared radiation treatment, filtering and collecting the filtrate, and finally subjecting the filtrate to low temperature concentration treatment to obtain the propolis water extract.

[0050] Embodiment 3:

[0051] (1) Using propolis propolis as raw material, first freezing it at -20°C for 12 hours; then crushing it, and then passing it through a 5-mesh sieve to obtain propolis particles;

[0052] (2) Add the material obtained in step (1) into an extraction kettle, using carbon dioxide as the fluid, CO 2The flow rate was 6L / min; the extraction pressure was adjusted to 25Mpa, the temperature was 35℃, and the time was 40min. Supercritical carbon dioxide extraction was performed and the CO was vented after extraction. 2 , complete the extraction and collect the residue after extraction, record it as the residue, and set it aside;

[0053] (3) adding the raffinate obtained in step (2) into water, wherein the ratio of the raffinate to the water is 1 g:4 mL; stirring evenly, performing ultrahigh pressure treatment, wherein the pressure is 350 MPa, the temperature is 30° C., the pressure holding time is 8 min, and the pressure is repeatedly increased and released 3 times to obtain an ultrahigh pressure treatment liquid;

[0054] (4) subjecting the ultrahigh pressure treated liquid obtained in step (3) to catalytic infrared radiation treatment, wherein the radiation temperature is 85° C., the radiation distance is 40 cm, and the action time is 4 min; after the catalytic infrared radiation treatment, filtering and collecting the filtrate, and finally subjecting the filtrate to low temperature concentration treatment to obtain the propolis water extract.

[0055] Verification results:

[0056] 1. Sensory testing:

[0057] Example 1 Samples of propolis water extracts Figure 1 As shown: It appears as brown to dark brown powder and has the unique aromatic smell of propolis.

[0058] 2. Water solubility test:

[0059] The water solubility of propolis water extract is tested in the following three aspects:

[0060] (1) After the aqueous solution is left to stand, observe whether an oil film is formed on the surface;

[0061] (2) After shaking the container, observe whether there are particles adhering to the container wall;

[0062] (3) Determine water solubility through visual inspection and sensory test.

[0063] The propolis water extracts of Examples 1-3 were added into deionized water at a mass ratio of 1:10. It was found that no oil film was formed on the surface of the propolis water extracts obtained by the above extraction method, and no particles adhered to the inner wall of the container after shaking the container. Visual inspection revealed that the propolis water extracts were completely and evenly dispersed in the water without precipitation, indicating that the propolis water extracts had excellent water solubility.

[0064] 3. GC-MS spectrum and determination of 12 phenolic compounds:

[0065] The propolis water extract of Example 1 was used as a sample, and volatile components were detected by GC-MS. Figure 2is a chromatogram; the content of phenolic compounds was detected according to GB / T 19427-2022 "Determination of the content of 12 phenolic compounds in propolis by liquid chromatography-tandem mass spectrometry and liquid chromatography", and the test results are shown in Table 1. Through qualitative and quantitative analysis of 12 polyphenolic components, the results showed that propolis water extract is rich in a variety of polyphenolic components, including flavonoids and phenolic acids. Specifically, flavonoids include brevipine-3-acetate, pinosylvin, galangin, cohen, etc.; phenolic acid compounds include caffeic acid, p-coumaric acid and ferulic acid. These polyphenols, as the main active ingredients in propolis, have multiple physiological functions such as antioxidant, antibacterial, anti-inflammatory and anti-tumor, indicating that they have great potential in development and application.

[0066]

[0067]

[0068] IV: Antibacterial test;

[0069] 1. The propolis water extract of Example 1 was used as a sample, and the sample was added into deionized water at a mass ratio of 1:15, and the sample was tested as a stock solution; deionized water was used as a control.

[0070] 2. Strain names: Escherichia coli (8099), Staphylococcus aureus (ATCC 6538), Candida albicans (ATCC10231).

[0071] 3. Inspection basis: Appendix CC1, C4 of GB 15979-2002 "Hygiene Standard for Disposable Sanitary Products";

[0072] 4.The test results are shown in Table 2.

[0073]

[0074] Five: Product application test example:

[0075] Test Example 1. Propolis Mouthwash

[0076] The propolis water extract of Example 1 was used as a sample and added into the formula in an amount of 6% to prepare a mouthwash. The formula of the mouthwash is shown in Table 3 below.

[0077] Element Mass fraction (%) Sorbitol 8 glycerin 6 Propolis water extract 6 Patchouli Honey 3 Poloxamer 407 1 Xylitol 1 Hydrogenated castor oil 0.2 Soybean Peptide 1 Menthol lactate 0.03 Honeysuckle Extract 1 Licorice Extract 1 essence 0.05 Potassium Sorbate 0.3 Deionized water margin

[0078] S1. Oral test without swallowing: Take 25 mL of mouthwash and put it directly in your mouth to feel the state of the mouthwash in your mouth;

[0079] The results showed that the mouthwash had no sticky feeling in the mouth, no odor, and no irritation to the mouth.

[0080] S2. Test on the antibacterial effect of mouthwash on three periodontal pathogens:

[0081] 1. Strain names: Fusobacterium nucleatum subsp. polmorphum ATCC 10953; Aetinobacillus actinomycetemicomilans ATCC 43717; Porphyromonas gingialis ATCC BAA-308.

[0082] 2. The detection method refers to WS / T 650-2019 (5.1.1).

[0083] 3.The test results are shown in Table 4.

[0084]

[0085]

[0086] It can be seen from the above table that the propolis mouthwash prepared in the test example of the present invention has a good antibacterial rate against Fusobacterium nucleatum polymorpha, Actinobacillus actinomycetemcomitans and Porphyromonas denticola.

[0087] Test Example 2. Propolis antibacterial oral spray

[0088] The propolis water extract of Example 1 was used as a sample and added into the formula in an amount of 8% to prepare a propolis antibacterial oral spray.

[0089] The formula of propolis antibacterial oral spray is shown in Table 5.

[0090] Element Mass fraction (%) Propolis water extract 8 Patchouli Honey 6 Honeysuckle Extract 3 Monk Fruit Extract 2 Peppermint Extract 2 Deionized water margin

[0091] Antibacterial test of propolis antibacterial oral spray;

[0092] 1. Strain names: Escherichia coli (8099), Staphylococcus aureus (ATCC 6538), Candida albicans (ATCC10231).

[0093] 2. Inspection basis: Appendix C C1, C4 of GB 15979-2002 "Hygiene Standard for Disposable Sanitary Products";

[0094] 3.The test results are shown in Table 6.

[0095]

[0096]

[0097] It can be seen from the above table that the propolis antibacterial oral spray prepared in the test example of the present invention has a good antibacterial rate against Escherichia coli, Staphylococcus aureus and Candida albicans.

[0098] In summary, the present invention uses water as the extraction solvent of the residue, combined with ultra-high pressure and catalytic infrared radiation treatment, thereby providing a more efficient, faster, safer and more economical extraction process. Moreover, the present invention can also prevent non-polar residues in the structure of raw propolis that may come from nature or human intervention from entering the final extract by using water as a solvent in the preparation process of propolis extract; the propolis water extract finally obtained is rich in a variety of active ingredients and is safe and odorless, and has good antibacterial properties. The propolis mouthwash in the product application test example has an inhibition rate of more than 94% against polymorphic subspecies of Fusobacterium nucleatum, Actinobacillus actinomycetemcomitans, and Porphyromonas denticola; the propolis antibacterial oral spray has an inhibition rate of more than 99.9% against Escherichia coli, Staphylococcus aureus, and Candida albicans, respectively; it shows that the propolis water extract of the present invention can be used in the preparation of oral care products.

[0099] Note: The above embodiments are only used to illustrate the present invention and are not intended to limit the technical solutions described in the present invention; therefore, although this specification has described the present invention in detail with reference to the above embodiments, a person skilled in the art should understand that the present invention can still be modified or replaced by equivalents; and all technical solutions and improvements thereof that do not depart from the spirit and scope of the present invention should be covered by the scope of the claims of the present invention.

Claims

1. A water extraction process for propolis supercritical extract residue, characterized in that: Here are the steps: (1) Using propolis propolis as a raw material, first freezing the propolis, then crushing it, and then sieving it to obtain propolis particles; (2) adding the wool rubber particles obtained in step (1) into an extraction kettle, using carbon dioxide as a fluid, and a CO2 flow rate of 6-8 L / min; and adjusting the extraction pressure to 25-30 MPa, the temperature to 30-50° C., and the time to 30-60 min, to perform supercritical carbon dioxide extraction, exhausting CO2 after extraction, completing the extraction and collecting the residue after extraction, which is recorded as the extract residue and set aside; (3) adding the raffinate obtained in step (2) into water, stirring evenly and then subjecting to ultra-high pressure treatment, the pressure is 250-350 MPa, the temperature is 30° C.-40° C., the pressure holding time is 5-8 min, and the pressure is repeatedly increased and released several times to obtain an ultra-high pressure treated liquid; (4) subjecting the ultrahigh pressure treated liquid obtained in step (3) to catalytic infrared radiation treatment, filtering and collecting the filtrate after the catalytic infrared radiation treatment, and finally subjecting the filtrate to low temperature concentration treatment to obtain a propolis water extract.

2. The water extraction process of a propolis supercritical extract residue according to claim 1, characterized in that: The temperature of the freezing treatment in step (1) is -20°C to -5°C, and the time is 8-12 hours; the mesh size of the sieve after crushing is 5-10 meshes.

3. The water extraction process of a propolis supercritical extract residue according to claim 1, characterized in that: The extraction temperature in step (2) is 35-40°C.

4. The water extraction process of a propolis supercritical extract residue according to claim 1, characterized in that: In step (3), the ratio of the amount of the raffinate to the amount of water is 1 g: 2-10 mL.

5. The water extraction process of a propolis supercritical extract residue according to claim 4, characterized in that: In step (3), the pressure increase and pressure relief in step 2 are repeated 2 to 3 times.

6. The water extraction process of a propolis supercritical extract residue according to claim 1, characterized in that: The radiation temperature in step (4) is 65 to 85° C., the radiation distance is 25 to 40 cm, and the action time is 2 to 10 minutes.

7. Use of the water extract prepared by the water extraction process according to any one of claims 1 to 6 for antibacterial purposes.

8. An oral care product, characterized in that: The oral care product comprises a water extract prepared by the water extraction process according to any one of claims 1 to 6; the oral care product comprises a mouthwash and an oral spray.

9. The oral care product according to claim 8, characterized in that: The cavity care product is propolis mouthwash, and the components are as follows: Sorbitol 8-10%, glycerin 4-6%, propolis aqueous extract 6-10%, patchouli honey 3-5%, poloxamer 4071-2%, xylitol 1-2%, hydrogenated castor oil 0.2-0.4%, soybean polypeptide 1-2%, menthyl lactate 0.03-0.05%, honeysuckle extract 1-2%, licorice extract 1-2%, essence 0.03-0.05%, potassium sorbate 0.3-0.5%, deionized water balance.

10. The oral care product according to claim 8, characterized in that: The cavity care product is a propolis antibacterial oral spray, and the components are as follows: Propolis water extract 8-10%, Patchouli 4-6%, Honeysuckle extract 3-5%, Monk Fruit extract 2-4%, Peppermint extract 2-4%, and deionized water as the balance.

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