Skin repair and whitening dressing based on black-skinned fir extract and preparation method

A skin dressing using black-skinned fir extract and a specific formulation enhances antibacterial properties and wound healing, addressing the limitations of existing dressings by providing long-lasting efficacy and skin whitening.

CN118873722BActive Publication Date: 2024-12-13INST OF URBAN AGRI CHINESE ACADEMY OF AGRI SCI
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Patent Information

Application Number
CN202411388209.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-08
Publication Date
2024-12-13
Estimated Expiration
2044-10-08

AI Technical Summary

Technical Problem

Existing skin dressings lack sufficient antibacterial properties, require frequent changes, have short antibacterial effects, and struggle to promote wound healing, while relying heavily on synthetic substances.

Method used

A skin dressing prepared using black-skinned fir extract, combining sodium hyaluronate, citrate pectin, and liposomes loaded with antimicrobial substances from black-skinned Acanthopanax chinensis and Citrus chinensis peel extracts, along with magnesium chloride, acrylamide, and N,N-methylenebisacrylamide to form a gel.

Benefits of technology

The dressing achieves high tyrosinase inhibition, long-lasting antibacterial effects, and promotes wound healing, with improved skin whitening and repair capabilities.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the technical field of skin dressings. The present invention provides a skin repair and whitening dressing based on a black-skinned spruce extract and a preparation method. The preparation method comprises the steps of: preparing a modified sodium hyaluronate solution by mixing citrine pectin with sodium hyaluronate; encapsulating a black-skinned spruce water extract dry powder, a black-skinned spruce ethanol aqueous solution extract dry powder and a citrine peel water extract in liposomes; and then placing the liposomes in a modified sodium hyaluronate solution to prepare a hydrogel colloid to obtain a dressing. The skin dressing obtained by the present invention can significantly inhibit tyrosinase and has a good scavenging rate for DPPH free radicals, and has a positive effect on skin whitening; at the same time, it also has excellent long-term antibacterial properties and can be used repeatedly for a long time; and it is also conducive to the repair and healing of burned skin.
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Description

Technical Field

[0001] The invention belongs to the technical field of skin dressings, and particularly relates to a skin repairing and whitening dressing based on a black-skinned fir extract and a preparation method thereof. Background Art

[0002] Skin is an important barrier that protects the human body from harmful external substances. Damage to the skin can cause a series of health and beauty problems, such as infection, accelerated progression of multiple chronic diseases, and facial appearance. In order to protect the skin, promote the healing of damaged skin, or improve skin quality, people have developed a variety of skin dressings, such as gauze, impregnated gauze, film dressings, foam dressings, and hydrogel dressings. For related content, see the summary of the literature "Application of Clinical Dressings in Skin Trauma".

[0003] At present, people have developed a variety of products in the above-mentioned skin dressing types and beauty products. However, the shortcomings of related products are mainly reflected in: (1) insufficient antibacterial properties, resulting in excessive use of antibacterial substances. For example, in order to achieve a 67.37% inhibition rate of tyrosinase in the "Preparation and Performance Evaluation of Antioxidant and Whitening Scutellaria Mud Mask", the amount of Scutellaria baicalensis extract added was as high as 40%; (2) it is difficult to prepare skin dressings with strong antibacterial properties using natural products; (3) the antibacterial effect of the dressing is short, and the dressing needs to be changed frequently; (4) the dressing is difficult to promote the healing of wounded skin.

[0004] The inventor of the present invention has long studied the biomedical uses of natural substances, and in recent years has focused on the development of black-skinned chicken mushroom. As far as the inventor knows, the current research on black-skinned chicken mushroom mainly focuses on its edible value, cultivation technology, antioxidant properties of extracts, etc., and there is little research on the antibacterial properties of its related components. At the same time, there is no report on its use in the preparation of skin dressings.

[0005] Therefore, whether it is possible to prepare a dressing based on the related substances of black-skinned chicken mushroom that has high and long-term antibacterial properties and also has the function of whitening skin and promoting the healing of wounded skin is a meaningful and challenging research. Summary of the invention

[0006] In view of the defects of the prior art, the object of the present invention is to provide a method for preparing a skin dressing having a high tyrosinase inhibition rate and good antioxidant properties, thereby exerting a skin whitening effect and also having the function of repairing damaged skin. On this basis, the object is also to use black-skinned Alpinia fasciata as a raw material to realize the high-value development of black-skinned Alpinia fasciata.

[0007] The present invention provides the following technical solutions to achieve the above-mentioned purpose.

[0008] A method for preparing a skin repairing and whitening dressing based on a black-skinned fir extract, characterized in that the preparation method comprises the following steps:

[0009] (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 3 to 5:1, dissolving in water, and preparing a solution having a citrate pectin weight content of 5 to 8 mg / mL;

[0010] (2) Preparing liposomes loaded with antimicrobial substances: using monostearate glyceryl, corn oil, soybean lecithin and Tween 80 as carrier materials for preparing liposomes, and using dried powder of water extract of black-skinned Acanthopanax chinensis, dried powder of ethanol aqueous solution extract of black-skinned Acanthopanax chinensis and water extract of Citrus chinensis peel in a weight ratio of 8:3:2-4 as antimicrobial substances for preparing liposomes; placing the antimicrobial substance in the carrier material and stirring it, and then subjecting it to high-pressure homogenization treatment to obtain liposomes loaded with antimicrobial substances;

[0011] (3) adding the antibacterial-loaded liposomes to the modified sodium hyaluronate solution at a weight ratio of 1:8-10, then adding magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stirring to dissolve, then adding ammonium persulfate and continuing to stir, and then forming a gel in a mold to obtain the dressing;

[0012] The citrine pectin is prepared from the peeled pulp of citrine fruit by utilizing a hydrothermal gelling method.

[0013] Preferably, the preparation method of the citrine pectin is: peel the citrine fruit and take out the pulp, chop it into puree, add water 5 times the weight of the puree, boil it at 90°C for 3 hours, filter and discard the puree, let it stand, take the lower sediment, remove impurities in the sediment with hot water, and finally dry it to obtain the citrine pectin.

[0014] Preferably, in step (2), the weight ratio of glyceryl monostearate, corn oil, soybean lecithin and Tween 80 is 6:4:6:3; and the weight ratio of the antibacterial substance to the carrier material is 1-1.5:100.

[0015] Preferably, in step (2), the monostearate glyceryl, corn oil, soybean lecithin and Tween 80 are mixed, heated to 80°C and stirred evenly; then the antibacterial substance is added and stirred at 80°C until dissolved; then water at 80°C is slowly added and stirred to obtain a pre-emulsion; and then the pre-emulsion is subjected to high-pressure homogenization.

[0016] Preferably, the preparation method of the black-skinned Alpinia chordata water extract is as follows: fresh black-skinned Alpinia chordata is washed, sliced, dried and powdered, the fungus powder is added to water at a solid-liquid weight ratio of 1:15, first extracted at 70°C for 2 hours, then heated to 100°C for extraction for 1 hour, centrifuged to remove residue, and the supernatant is concentrated under reduced pressure to obtain a paste, which is then freeze-dried to obtain dry powder; the preparation method of the Huangjing fruit peel water extract is as follows: Huangjing fruit is washed and peeled, the peel is chopped and dried, the dried peel is added to water at a solid-liquid weight ratio of 1:10, first extracted at 80°C for 3 hours, then heated to 90°C for extraction for 1 hour, centrifuged to remove residue, the supernatant is concentrated under reduced pressure to obtain a paste, which is then freeze-dried to obtain dry powder.

[0017] Preferably, the preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia choristae is: fresh black-skinned Alpinia choristae is washed, sliced, dried and powdered, the bacterial powder is added to a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 according to a solid-liquid weight ratio of 1:10, extracted at 50°C for 5 hours, centrifuged, and the supernatant was concentrated under reduced pressure to obtain a paste, which was then freeze-dried to obtain dry powder. Freeze-drying to obtain dry powder.

[0018] Preferably, in step (3), the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when magnesium chloride is added, the concentration of the added magnesium chloride solution is 1 M, and the volume-to-weight ratio of the magnesium chloride solution to sodium hyaluronate is 5 mL:1 g.

[0019] Preferably, in step (1), sodium hyaluronate and citrate pectin are mixed in a weight ratio of 4:1 and dissolved in water to prepare a solution with a citrate pectin weight content of 6 mg / mL.

[0020] Preferably, in step (2), the weight ratio of the dry powder of the water extract of Acanthopanax nigra, the dry powder of the ethanol aqueous solution extract of Acanthopanax nigra and the water extract of Citrina chinensis peel is 8:3:3; in step (3), the weight ratio of the liposome loaded with the antibacterial substance to the modified sodium hyaluronate solution is 1:9.

[0021] Another object of the present invention is to provide a skin repairing and whitening dressing based on the black-skinned Fir extract prepared by the above preparation method.

[0022] Beneficial effects of the present invention:

[0023] The skin dressing obtained by the invention can significantly inhibit tyrosinase and has a good scavenging rate for DPPH free radicals, and has a positive effect on skin whitening; at the same time, it also has excellent long-term antibacterial properties, can be repeatedly used for a long time, and is also conducive to the repair and healing of burned skin. DETAILED DESCRIPTION

[0024] The present invention is described in detail below through examples. It is necessary to point out that the following examples are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by technical personnel in this field based on the above invention content still fall within the scope of protection of the present invention.

[0025] Example 1

[0026] Raw materials: black-skinned fir, commercially available; yellow crystal fruit, commercially available; sodium hyaluronate, M W =2000kDa, Xi'an Baichuan Biotechnology Co., Ltd.; glyceryl monostearate, corn oil, soybean lecithin, Shaanxi Chenming Biotechnology Co., Ltd.; acrylamide, Shanghai Aladdin Biochemical Technology Co., Ltd.; N,N-methylenebisacrylamide, Chongqing Shuyi Technology Co., Ltd.; ammonium persulfate, Shanghai Tengzhun Biotechnology Co., Ltd.; Tween 80, Sinopharm Chemical Reagent Co., Ltd.; other chemical reagents were owned by the laboratory.

[0027] Preparation method:

[0028] (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 4:1, dissolving in water, and preparing a solution having a citrate pectin weight content of 6 mg / mL;

[0029] (2) Preparing liposomes loaded with antimicrobial substances: Glyceryl monostearate, corn oil, soybean lecithin and Tween 80 were mixed in a weight ratio of 6:4:6:3, heated to 80°C, and stirred evenly to obtain a carrier material; black-skinned Acanthopanax water extract dry powder, black-skinned Acanthopanax ethanol aqueous solution extract dry powder and Citrus chinensis peel water extract in a weight ratio of 8:3:3 were used as antimicrobial substances for preparing liposomes, and the carrier material was added, and continued to be stirred at 80°C until dissolved; then 80°C water was slowly added and stirred to obtain a pre-emulsion; then the pre-emulsion was subjected to high-pressure homogenization to obtain liposomes loaded with antimicrobial substances; wherein the weight ratio of the antimicrobial substance to the carrier material was 1.5:100;

[0030] (3) Add the antibacterial-loaded liposomes to the modified sodium hyaluronate solution at a weight ratio of 1:9, then add magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stir to dissolve, then add ammonium persulfate and continue stirring, and then gel in a mold to obtain the dressing; wherein the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when adding magnesium chloride, the concentration of the added magnesium chloride solution is 1 M, and the volume weight ratio of the magnesium chloride solution to the sodium hyaluronate is 5 mL:1 g.

[0031] The preparation method of citrine pectin is as follows: peel the citrine fruit, take out the pulp, chop and mash it into puree, add water 5 times the weight of the puree, boil it at 90°C for 3 hours, filter and discard the puree, let it stand, take out the lower sediment, remove impurities in the sediment with hot water, and finally dry it to obtain citrine pectin.

[0032] The preparation method of the black-skinned Acanthopanax water extract is as follows: fresh black-skinned Acanthopanax is washed, sliced, dried and powdered, the powder is added into water at a solid-liquid weight ratio of 1:15, the powder is first extracted at 70°C for 2 hours, then the temperature is raised to 100°C for extraction for 1 hour, the residue is removed by centrifugation, the supernatant is concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain dry powder.

[0033] The preparation method of the water extract of the yellow crystal fruit peel is as follows: wash and peel the yellow crystal fruit, chop the peel and dry it, add the dried peel into water according to a solid-liquid weight ratio of 1:10, first extract at 80°C for 3 hours, then heat to 90°C for extraction for 1 hour, centrifuge to remove the residue, take the supernatant and concentrate it under reduced pressure to obtain a paste, and then freeze-dry it to obtain a dry powder.

[0034] The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia chortensis is as follows: fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the fungus powder is added into a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, the extraction is carried out at 50°C for 5 hours, the supernatant is taken after centrifugation, and reduced pressure concentration is performed to obtain a paste, and then freeze-drying is performed to obtain dry powder. Freeze-drying is performed to obtain dry powder.

[0035] Example 2

[0036] The raw materials are consistent with those in Example 1.

[0037] Preparation method:

[0038] (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 3:1, dissolving in water, and preparing a solution having a citrate pectin weight content of 5 mg / mL;

[0039] (2) Preparing liposomes loaded with antibacterial substances: Glyceryl monostearate, corn oil, soybean lecithin and Tween 80 were mixed in a weight ratio of 6:4:6:3, heated to 80°C, and stirred evenly to obtain a carrier material; black-skinned Acanthopanax water extract dry powder, black-skinned Acanthopanax ethanol aqueous solution extract dry powder and Citrus chinensis peel water extract in a weight ratio of 8:3:4 were used as antibacterial substances for preparing liposomes, and the carrier material was added, and continued to be stirred at 80°C until dissolved; then 80°C water was slowly added and stirred to obtain a pre-emulsion; then the pre-emulsion was subjected to high-pressure homogenization to obtain liposomes loaded with antibacterial substances; wherein the weight ratio of the antibacterial substance to the carrier material was 1.2:100;

[0040] (3) Add the antibacterial-loaded liposomes to the modified sodium hyaluronate solution at a weight ratio of 1:10, then add magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stir to dissolve, then add ammonium persulfate and continue stirring, and then gel in a mold to obtain the dressing; wherein the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when adding magnesium chloride, the concentration of the added magnesium chloride solution is 1 M, and the volume weight ratio of the magnesium chloride solution to the sodium hyaluronate is 5 mL:1 g.

[0041] The preparation method of citrine pectin is as follows: peel the citrine fruit, take out the pulp, chop and mash it into puree, add water 5 times the weight of the puree, boil it at 90°C for 3 hours, filter and discard the puree, let it stand, take out the lower sediment, remove impurities in the sediment with hot water, and finally dry it to obtain citrine pectin.

[0042] The preparation method of the black-skinned Acanthopanax water extract is as follows: fresh black-skinned Acanthopanax is washed, sliced, dried and powdered, the powder is added into water at a solid-liquid weight ratio of 1:15, the powder is first extracted at 70°C for 2 hours, then the temperature is raised to 100°C for extraction for 1 hour, the residue is removed by centrifugation, the supernatant is concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain dry powder.

[0043] The preparation method of the water extract of the yellow crystal fruit peel is as follows: wash and peel the yellow crystal fruit, chop the peel and dry it, add the dried peel into water according to a solid-liquid weight ratio of 1:10, first extract at 80°C for 3 hours, then heat to 90°C for extraction for 1 hour, centrifuge to remove the residue, take the supernatant and concentrate it under reduced pressure to obtain a paste, and then freeze-dry it to obtain a dry powder.

[0044] The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia chortensis is as follows: fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the fungus powder is added into a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, the extraction is carried out at 50°C for 5 hours, the supernatant is taken after centrifugation, and reduced pressure concentration is performed to obtain a paste, and then freeze-drying is performed to obtain dry powder. Freeze-drying is performed to obtain dry powder.

[0045] Example 3

[0046] The raw materials are consistent with those in Example 1.

[0047] Preparation method:

[0048] (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 5:1, dissolving in water, and preparing a solution with a citrate pectin weight content of 8 mg / mL;

[0049] (2) Preparing liposomes loaded with antibacterial substances: Glyceryl monostearate, corn oil, soybean lecithin and Tween 80 are mixed in a weight ratio of 6:4:6:3, heated to 80°C, and stirred evenly to obtain a carrier material; black-skinned Acanthopanax water extract dry powder, black-skinned Acanthopanax ethanol aqueous solution extract dry powder and Citrus chinensis peel water extract in a weight ratio of 8:3:2 are used as antibacterial substances for preparing liposomes, and the carrier material is added, and stirring is continued at 80°C until dissolved; then 80°C water is slowly added and stirred to obtain a pre-emulsion; then the pre-emulsion is subjected to high-pressure homogenization to obtain liposomes loaded with antibacterial substances; wherein the weight ratio of the antibacterial substance to the carrier material is 1:100;

[0050] (3) Add the antibacterial-loaded liposomes to the modified sodium hyaluronate solution at a weight ratio of 1:8, then add magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stir to dissolve, then add ammonium persulfate and continue stirring, and then gel in a mold to obtain the dressing; wherein the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when adding magnesium chloride, the concentration of the added magnesium chloride solution is 1 M, and the volume weight ratio of the magnesium chloride solution to the sodium hyaluronate is 5 mL:1 g.

[0051] The preparation method of citrine pectin is as follows: peel the citrine fruit, take out the pulp, chop and mash it into puree, add water 5 times the weight of the puree, boil it at 90°C for 3 hours, filter and discard the puree, let it stand, take out the lower sediment, remove impurities in the sediment with hot water, and finally dry it to obtain citrine pectin.

[0052] The preparation method of the black-skinned Acanthopanax water extract is as follows: fresh black-skinned Acanthopanax is washed, sliced, dried and powdered, the powder is added into water at a solid-liquid weight ratio of 1:15, the powder is first extracted at 70°C for 2 hours, then the temperature is raised to 100°C for extraction for 1 hour, the residue is removed by centrifugation, the supernatant is concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain dry powder.

[0053] The preparation method of the water extract of the yellow crystal fruit peel is as follows: wash and peel the yellow crystal fruit, chop the peel and dry it, add the dried peel into water according to a solid-liquid weight ratio of 1:10, first extract at 80°C for 3 hours, then heat to 90°C for extraction for 1 hour, centrifuge to remove the residue, take the supernatant and concentrate it under reduced pressure to obtain a paste, and then freeze-dry it to obtain a dry powder.

[0054] The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia chortensis is as follows: fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the fungus powder is added into a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, the extraction is carried out at 50°C for 5 hours, the supernatant is taken after centrifugation, and reduced pressure concentration is performed to obtain a paste, and then freeze-drying is performed to obtain dry powder. Freeze-drying is performed to obtain dry powder.

[0055] Comparative Example 1

[0056] The raw materials are the same as those in Example 1. Except that yellow crystal fruit pectin is not added, the rest is the same as in Example 1.

[0057] Preparation method:

[0058] (1) Preparing a sodium hyaluronate solution: dissolving sodium hyaluronate in water to prepare a solution having a sodium hyaluronate weight content of 24 mg / mL;

[0059] (2) Preparing liposomes loaded with antimicrobial substances: Glyceryl monostearate, corn oil, soybean lecithin and Tween 80 were mixed in a weight ratio of 6:4:6:3, heated to 80°C, and stirred evenly to obtain a carrier material; black-skinned Acanthopanax water extract dry powder, black-skinned Acanthopanax ethanol aqueous solution extract dry powder and Citrus chinensis peel water extract in a weight ratio of 8:3:3 were used as antimicrobial substances for preparing liposomes, and the carrier material was added, and continued to be stirred at 80°C until dissolved; then 80°C water was slowly added and stirred to obtain a pre-emulsion; then the pre-emulsion was subjected to high-pressure homogenization to obtain liposomes loaded with antimicrobial substances; wherein the weight ratio of the antimicrobial substance to the carrier material was 1.5:100;

[0060] (3) Add the antibacterial-loaded liposomes to a sodium hyaluronate solution at a weight ratio of 1:9, then add magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stir to dissolve, then add ammonium persulfate and continue stirring, and then gel in a mold to obtain the dressing; wherein the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when adding magnesium chloride, the concentration of the added magnesium chloride solution is 1 M, and the volume weight ratio of the magnesium chloride solution to the sodium hyaluronate is 5 mL:1 g.

[0061] The preparation method of the black-skinned Acanthopanax water extract is as follows: fresh black-skinned Acanthopanax is washed, sliced, dried and powdered, the powder is added into water at a solid-liquid weight ratio of 1:15, the powder is first extracted at 70°C for 2 hours, then the temperature is raised to 100°C for extraction for 1 hour, the residue is removed by centrifugation, the supernatant is concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain dry powder.

[0062] The preparation method of the water extract of the yellow crystal fruit peel is as follows: wash and peel the yellow crystal fruit, chop the peel and dry it, add the dried peel into water according to a solid-liquid weight ratio of 1:10, first extract at 80°C for 3 hours, then heat to 90°C for extraction for 1 hour, centrifuge to remove the residue, take the supernatant and concentrate it under reduced pressure to obtain a paste, and then freeze-dry it to obtain a dry powder.

[0063] The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia chortensis is as follows: fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the fungus powder is added into a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, the extraction is carried out at 50°C for 5 hours, the supernatant is taken after centrifugation, and reduced pressure concentration is performed to obtain a paste, and then freeze-drying is performed to obtain dry powder. Freeze-drying is performed to obtain dry powder.

[0064] Comparative Example 2

[0065] The raw materials are consistent with those in Example 1.

[0066] Except that the addition ratio of sodium hyaluronate to citrate pectin is 2:1, the preparation method is the same as that of Example 1, specifically:

[0067] (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 2:1, dissolving in water, and preparing a solution having a citrate pectin weight content of 6 mg / mL;

[0068] (2) Preparing liposomes loaded with antimicrobial substances: Glyceryl monostearate, corn oil, soybean lecithin and Tween 80 were mixed in a weight ratio of 6:4:6:3, heated to 80°C, and stirred evenly to obtain a carrier material; black-skinned Acanthopanax water extract dry powder, black-skinned Acanthopanax ethanol aqueous solution extract dry powder and Citrus chinensis peel water extract in a weight ratio of 8:3:3 were used as antimicrobial substances for preparing liposomes, and the carrier material was added, and continued to be stirred at 80°C until dissolved; then 80°C water was slowly added and stirred to obtain a pre-emulsion; then the pre-emulsion was subjected to high-pressure homogenization to obtain liposomes loaded with antimicrobial substances; wherein the weight ratio of the antimicrobial substance to the carrier material was 1.5:100;

[0069] (3) Add the antibacterial-loaded liposomes to the modified sodium hyaluronate solution at a weight ratio of 1:9, then add magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stir to dissolve, then add ammonium persulfate and continue stirring, and then gel in a mold to obtain the dressing; wherein the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when adding magnesium chloride, the concentration of the added magnesium chloride solution is 1 M, and the volume weight ratio of the magnesium chloride solution to the sodium hyaluronate is 5 mL:1 g.

[0070] The preparation method of citrine pectin is as follows: peel the citrine fruit, take out the pulp, chop and mash it into puree, add water 5 times the weight of the puree, boil it at 90°C for 3 hours, filter and discard the puree, let it stand, take out the lower sediment, remove impurities in the sediment with hot water, and finally dry it to obtain citrine pectin.

[0071] The preparation method of the black-skinned Acanthopanax water extract is as follows: fresh black-skinned Acanthopanax is washed, sliced, dried and powdered, the powder is added into water at a solid-liquid weight ratio of 1:15, the powder is first extracted at 70°C for 2 hours, then the temperature is raised to 100°C for extraction for 1 hour, the residue is removed by centrifugation, the supernatant is concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain dry powder.

[0072] The preparation method of the water extract of the yellow crystal fruit peel is as follows: wash and peel the yellow crystal fruit, chop the peel and dry it, add the dried peel into water according to a solid-liquid weight ratio of 1:10, first extract at 80°C for 3 hours, then heat to 90°C for extraction for 1 hour, centrifuge to remove the residue, take the supernatant and concentrate it under reduced pressure to obtain a paste, and then freeze-dry it to obtain a dry powder.

[0073] The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia chortensis is as follows: fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the fungus powder is added into a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, the extraction is carried out at 50°C for 5 hours, the supernatant is taken after centrifugation, and reduced pressure concentration is performed to obtain a paste, and then freeze-drying is performed to obtain dry powder. Freeze-drying is performed to obtain dry powder.

[0074] Comparative Example 3

[0075] The raw materials are consistent with those in Example 1.

[0076] Except that the addition ratio of sodium hyaluronate to citrate pectin is 8:1, the preparation method is the same as that of Example 1, specifically:

[0077] (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 8:1, dissolving in water, and preparing a solution having a citrate pectin weight content of 6 mg / mL;

[0078] (2) Preparing liposomes loaded with antimicrobial substances: Glyceryl monostearate, corn oil, soybean lecithin and Tween 80 were mixed in a weight ratio of 6:4:6:3, heated to 80°C, and stirred evenly to obtain a carrier material; black-skinned Acanthopanax water extract dry powder, black-skinned Acanthopanax ethanol aqueous solution extract dry powder and Citrus chinensis peel water extract in a weight ratio of 8:3:3 were used as antimicrobial substances for preparing liposomes, and the carrier material was added, and continued to be stirred at 80°C until dissolved; then 80°C water was slowly added and stirred to obtain a pre-emulsion; then the pre-emulsion was subjected to high-pressure homogenization to obtain liposomes loaded with antimicrobial substances; wherein the weight ratio of the antimicrobial substance to the carrier material was 1.5:100;

[0079] (3) Add the antibacterial-loaded liposomes to the modified sodium hyaluronate solution at a weight ratio of 1:9, then add magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stir to dissolve, then add ammonium persulfate and continue stirring, and then gel in a mold to obtain the dressing; wherein the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when adding magnesium chloride, the concentration of the added magnesium chloride solution is 1 M, and the volume weight ratio of the magnesium chloride solution to the sodium hyaluronate is 5 mL:1 g.

[0080] The preparation method of citrine pectin is as follows: peel the citrine fruit, take out the pulp, chop and mash it into puree, add water 5 times the weight of the puree, boil it at 90°C for 3 hours, filter and discard the puree, let it stand, take out the lower sediment, remove impurities in the sediment with hot water, and finally dry it to obtain citrine pectin.

[0081] The preparation method of the black-skinned Acanthopanax water extract is as follows: fresh black-skinned Acanthopanax is washed, sliced, dried and powdered, the powder is added into water at a solid-liquid weight ratio of 1:15, the powder is first extracted at 70°C for 2 hours, then the temperature is raised to 100°C for extraction for 1 hour, the residue is removed by centrifugation, the supernatant is concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain dry powder.

[0082] The preparation method of the water extract of the yellow crystal fruit peel is as follows: wash and peel the yellow crystal fruit, chop the peel and dry it, add the dried peel into water according to a solid-liquid weight ratio of 1:10, first extract at 80°C for 3 hours, then heat to 90°C for extraction for 1 hour, centrifuge to remove the residue, take the supernatant and concentrate it under reduced pressure to obtain a paste, and then freeze-dry it to obtain a dry powder.

[0083] The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia chortensis is as follows: fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the fungus powder is added into a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, the extraction is carried out at 50°C for 5 hours, the supernatant is taken after centrifugation, and reduced pressure concentration is performed to obtain a paste, and then freeze-drying is performed to obtain dry powder. Freeze-drying is performed to obtain dry powder.

[0084] Comparative Example 4

[0085] The following substances were prepared according to weight percentage: 1% fish collagen, 5% antibacterial substance of Example 1, 0.3% sodium hyaluronate, 2% 1,3-propylene glycol, 0.1% phenoxyethanol, and the balance was deionized water.

[0086] (1) Add fish collagen, sodium hyaluronate and 1,3-propylene glycol to three-fifths of deionized water and stir evenly to obtain solution A;

[0087] (2) then adding the antibacterial substance in Example 1, adding the remaining deionized water, stirring, and then treating at 80° C. for 45 minutes to obtain solution B;

[0088] (3) After cooling solution B to room temperature, add it to solution A, and then add phenoxyethanol and stir;

[0089] (4) The product obtained in step (3) is coated on a non-woven fabric to obtain a skin dressing.

[0090] Comparative Example 5

[0091] The raw materials used are consistent with those in Example 1.

[0092] The preparation method is consistent with Example 1 except that the antibacterial substance is directly added, specifically:

[0093] (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 4:1, dissolving in water, and preparing a solution having a citrate pectin weight content of 6 mg / mL;

[0094] (2) Using a weight ratio of 8:3:3 of dried powder of water extract of Hei Pi Jun Feng, dried powder of ethanol aqueous solution extract of Hei Pi Jun Feng, and water extract of Huang Jing fruit peel as antibacterial agents for later use;

[0095] (3) Add the antibacterial substance to the modified sodium hyaluronate solution at a weight ratio of 1:9, then add magnesium chloride, acrylamide and N,N-methylenebisacrylamide and stir to dissolve, then add ammonium persulfate and continue stirring, and then gel in a mold to obtain the dressing; wherein the added amounts of acrylamide, N,N-methylenebisacrylamide and ammonium persulfate are 2 times, 0.05 times and 0.1 times the weight of sodium hyaluronate, respectively; when adding magnesium chloride, the concentration of the added magnesium chloride solution is 1 M, and the volume weight ratio of the magnesium chloride solution to the sodium hyaluronate is 5 mL:1 g.

[0096] The preparation method of citrine pectin is as follows: peel the citrine fruit, take out the pulp, chop and mash it into puree, add water 5 times the weight of the puree, boil it at 90°C for 3 hours, filter and discard the puree, let it stand, take out the lower sediment, remove impurities in the sediment with hot water, and finally dry it to obtain citrine pectin.

[0097] The preparation method of the black-skinned Acanthopanax water extract is as follows: fresh black-skinned Acanthopanax is washed, sliced, dried and powdered, the powder is added into water at a solid-liquid weight ratio of 1:15, the powder is first extracted at 70°C for 2 hours, then the temperature is raised to 100°C for extraction for 1 hour, the residue is removed by centrifugation, the supernatant is concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain dry powder.

[0098] The preparation method of the water extract of the yellow crystal fruit peel is as follows: wash and peel the yellow crystal fruit, chop the peel and dry it, add the dried peel into water according to a solid-liquid weight ratio of 1:10, first extract at 80°C for 3 hours, then heat to 90°C for extraction for 1 hour, centrifuge to remove the residue, take the supernatant and concentrate it under reduced pressure to obtain a paste, and then freeze-dry it to obtain a dry powder.

[0099] The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Alpinia chortensis is as follows: fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the fungus powder is added into a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, the extraction is carried out at 50°C for 5 hours, the supernatant is taken after centrifugation, and reduced pressure concentration is performed to obtain a paste, and then freeze-drying is performed to obtain dry powder. Freeze-drying is performed to obtain dry powder.

[0100] Experimental Example 1

[0101] Determination of tyrosinase inhibition rate: refer to the method of "Preparation and performance evaluation of antioxidant and whitening scutellaria mud mask" (DOI: 10.20099 / j.issn.1000-4475.2022.0161), but make some modifications. The specific scheme is as follows:

[0102] Take the dressings obtained in Examples 1 to 3 and Comparative Examples 1 to *, spray the dressings with ultrapure water evenly at a weight ratio of 1:1 and incubate at 36°C. Take 1 mL one hour later, add 0.9 mL of Tris (Tris) hydrochloric acid buffer with a pH of 7.6 and 1 mL of tyrosine with a mass fraction of 0.03% in a test tube, place in a constant temperature water bath at 37°C for 10 min, add 0.1 mL of tyrosinase aqueous solution (1070 U / mL), mix the solution evenly, and place in a constant temperature water bath at 37°C for 25 min. Calculate by measuring the absorbance with an ultraviolet spectrophotometer, see the document for details.

[0103] Determination of DPPH free radical scavenging rate: refer to the method of "Preparation and performance evaluation of antioxidant and whitening scutellaria mud mask" (DOI: 10.20099 / j.issn.1000-4475.2022.0161), but make some modifications. The specific scheme is as follows:

[0104] Take the dressings obtained in Examples 1 to 3 and Comparative Examples 1 to 5, spray ultrapure water evenly on the dressings at a weight ratio of 1:1 and incubate at 36°C. After one hour, take 1 mL and mix with 1 mL DPPH·solution (2×10 -8 mol / L), shake well and place in the dark for 30 min, measure the absorbance of each reaction solution at 517 nm, and calculate the scavenging rate of each sample for DPPH free radicals.

[0105] The experimental results of tyrosinase inhibition rate and DPPH free radical scavenging rate are shown in Table 1.

[0106] Table 1

[0107]

[0108] As shown in Table 1, the present invention has excellent effects on both tyrosinase inhibition rate and DPPH free radical scavenging rate. At the same time, it can also be seen that when the amount of yellow crystal fruit pectin added is too much, it has a significant impact on both tyrosinase inhibition rate and DPPH free radical scavenging rate.

[0109] Experimental Example 2

[0110] Determination of antibacterial activity: The dressings obtained in Examples 1 to 3 and Comparative Examples 1 to 5 were cut into samples with a length, width and height of 1 cm × 1 cm × 0.5 cm, and placed in 20 mL of a 1 × 10 7 cfu / mL of the tested bacteria (Staphylococcus aureus and Escherichia coli) were incubated at 37°C for 5 hours to test the antibacterial rate. After the incubation, the samples were washed with PBS and then placed in 20 mL of a 1×10 7cfu / mL of the tested bacteria (Staphylococcus aureus and Escherichia coli, respectively) were incubated for the second time to test the retention of the samples in terms of antibacterial properties. The test results are shown in Table 2.

[0111] Table 2

[0112]

[0113] As shown in Table 2, the addition of yellow crystal fruit pectin and the addition ratio play an important role in maintaining the antibacterial property and the antibacterial property. When sodium hyaluronate is mixed and modified without yellow crystal fruit pectin, the antibacterial property is difficult to maintain, and the reason may be that the antibiotic has been released suddenly and is difficult to release for a long time. At the same time, when the amount of yellow crystal fruit pectin added is too much, it will cause the antibiotic to be difficult to release effectively, affecting the antibacterial effect. At the same time, it can also be known that even if the antibiotic of the present invention is used as an active ingredient, but different dressing substrates are selected, there is also a huge impact on the antibacterial property. In addition, even if the ratio of each substance of the antibiotic is unchanged, sodium hyaluronate is also modified with yellow crystal fruit pectin, but the antibiotic is not encapsulated in liposomes, the maintenance effect of the antibacterial property will also decline significantly.

[0114] Experimental Example 3

[0115] Experiment on the repair effect of rat skin burns: 15 rats weighing 200-220g were used as test animals, and 5 rats were randomly assigned to each group. The burn model was constructed with reference to the literature "Establishing a new rat burn model by burning with paste solid alcohol". The dressing obtained in Example 1 was used as the experimental group, the vaseline gauze was used as the control group, and the untreated group was used as the model group. Each group was fixed with sterile gauze, and the dressing was changed every other day. The wound healing was recorded by taking pictures, and the time of dry scab shedding and new fur covering time were recorded. The experimental results are shown in Table 3.

[0116] Table 3

[0117]

[0118] As shown in Table 3, the present invention can accelerate the healing speed of burned skin.

[0119] Experimental Example 4

[0120] At the beginning of the research of the present invention, the inventor conducted preliminary experiments to examine the antibacterial effects of different extracts. Based on these experiments, the present invention was able to carry out further dressing preparation experiments. In order to better understand the present invention, the inventor introduces some of the previous research results in this regard.

[0121] The dried powder of water extract of Acanthopanax nigra, the dried powder of ethanol aqueous solution extract of Acanthopanax nigra and the water extract of Citrina chinensis peel were prepared as described in Example 1.

[0122] Black-skinned Alpinia chortensis petroleum ether extract: Fresh black-skinned Alpinia chortensis is washed, sliced, dried and powdered, the powder is added to petroleum ether at a solid-liquid weight ratio of 1:8, extracted at 80°C for 2 hours, concentrated under reduced pressure to obtain a paste, and then freeze-dried to obtain a dry powder.

[0123] The dry powder of water extract of Acanthopanax nigra, the dry powder of ethanol aqueous solution extract of Acanthopanax nigra, the petroleum ether extract of Acanthopanax nigra and the water extract of Huangjing fruit peel were freely mixed to form different experimental groups to investigate the effects on antibacterial properties.

[0124] Antibacterial experiment: 1 mg of dry powder from each group was added to 10 mL of PBS suspension of the tested bacteria (Staphylococcus aureus and Escherichia coli, respectively) (bacterial concentration was 1×10 9 cfu / mL) and incubated at 37°C for 5 hours to test the antibacterial rate. Some groups and antibacterial results are shown in Tables 4 and 5, respectively.

[0125] Table 4

[0126]

[0127] Note: The values ​​in the table are the added quantities of each substance.

[0128] Table 5

[0129]

[0130] As shown in Table 5, the water extract of Huangjing fruit peel has a synergistic effect with the dry powder of water extract of Hei Pi Jun Feng and the dry powder of ethanol aqueous solution extract of Hei Pi Jun Feng in terms of antibacterial effect, and the synergistic antibacterial effect also depends on the ratio of the three substances. At the same time, the petroleum ether extract of Hei Pi Jun Feng has a certain antagonistic effect on antibacterial activity in the corresponding experimental groups.

Claims

1. A method for preparing a skin repairing and whitening dressing based on a black-skinned fir extract, characterized in that: The preparation method comprises the following steps: (1) Preparing a modified sodium hyaluronate solution: mixing sodium hyaluronate and citrate pectin at a weight ratio of 3 to 5:1, dissolving the mixture in water, and preparing a solution having a citrate pectin weight content of 5 to 8 mg / mL; (2) Preparation of liposomes loaded with antimicrobial substances: monostearate, corn oil, soybean lecithin and Tween 80 were used as carrier materials for preparing liposomes, and dry powder of water extract of black-skinned Aconitum juncea, dry powder of ethanol aqueous solution extract of black-skinned Aconitum juncea and water extract of Citrus chinensis peel in a weight ratio of 8:3:2-4 were used as antimicrobial substances for preparing liposomes; the antimicrobial substance was placed in the carrier material and stirred, and then subjected to high-pressure homogenization to obtain liposomes loaded with antimicrobial substances; (3) adding the antibacterial-loaded liposomes to the modified sodium hyaluronate solution at a weight ratio of 1:8-10, then adding magnesium chloride, acrylamide, and N,N-methylenebisacrylamide and stirring to dissolve, then adding ammonium persulfate and continuing to stir, and then forming a gel in a mold to obtain the dressing; The citrine pectin is prepared from the peeled pulp of citrine fruit by utilizing a hydrothermal gelling method.

2. The method for preparing a skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 1, wherein: The preparation method of the citrine pectin comprises the following steps: peeling the citrine fruit, taking out the pulp, chopping and mashing the pulp into a puree, adding water 5 times the weight of the puree, boiling at 90° C. for 3 hours, filtering and discarding the puree, and then allowing the pulp to stand for a treatment. The lower sediment is taken out, and impurities in the sediment are removed with hot water. Finally, the pulp is dried to obtain the citrine pectin.

3. The method for preparing a skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 1, wherein: In step (2), the weight ratio of glyceryl monostearate, corn oil, soybean lecithin and Tween 80 is 6:4:6:3; the weight ratio of the antibacterial substance to the carrier material is 1~1.5:

100.

4. The method for preparing the skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 3, characterized in that: In step (2), the monostearate, corn oil, soybean lecithin and Tween 80 are mixed, heated to 80°C and stirred evenly; then the antibacterial substance is added and stirred at 80°C until dissolved; then 80°C water is slowly added and stirred to obtain a pre-emulsion; and then the pre-emulsion is subjected to high-pressure homogenization.

5. The method for preparing the skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 1, characterized in that: The preparation method of the black-skinned Aconitum albuminosa water extract dry powder is as follows: fresh black-skinned Aconitum albuminosa is washed, sliced, dried and powdered, the fungus powder is added to water at a solid-liquid weight ratio of 1:15, first extracted at 70°C for 2 hours, then heated to 100°C for extraction for 1 hour, centrifuged to remove residue, and the supernatant is concentrated under reduced pressure to obtain a paste, which is then freeze-dried to obtain dry powder; the preparation method of the yellow crystal peel water extract is as follows: yellow crystal fruit is washed and peeled, the peel is chopped and dried, the dried peel is added to water at a solid-liquid weight ratio of 1:10, first extracted at 80°C for 3 hours, then heated to 90°C for extraction for 1 hour, centrifuged to remove residue, and the supernatant is concentrated under reduced pressure to obtain a paste, which is then freeze-dried to obtain dry powder.

6. The method for preparing the skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 5, characterized in that: The preparation method of the dry powder of the ethanol aqueous solution extract of black-skinned Aconitum capsici mushroom comprises: washing, slicing, drying and powdering fresh black-skinned Aconitum capsici mushroom, adding the mushroom powder to a mixed solvent consisting of ethanol and water in a volume ratio of 3:2 at a solid-liquid weight ratio of 1:10, extracting at 50°C for 5 hours, taking the supernatant after centrifugation and concentrating under reduced pressure to obtain a paste, and then freeze-drying to obtain dry powder.

7. The method for preparing the skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 1, characterized in that: In step (3), the added amounts of acrylamide, N,N-methylenebisacrylamide, and ammonium persulfate are 2 times, 0.05 times, and 0.1 times the weight of sodium hyaluronate, respectively; when magnesium chloride is added, the concentration of the added magnesium chloride solution is 1 M, and the volume-to-weight ratio of the magnesium chloride solution to sodium hyaluronate is 5 mL:1 g.

8. The method for preparing the skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 1, characterized in that: In step (1), sodium hyaluronate and citrate pectin are mixed in a weight ratio of 4:1 and dissolved in water to prepare a solution having a citrate pectin weight content of 6 mg / mL.

9. The method for preparing the skin repairing and whitening dressing based on the extract of Aconitum carmichaelii according to claim 1, characterized in that: In step (2), the weight ratio of the dried powder of the water extract of Aconitum carmichaelii, the dried powder of the ethanol aqueous solution extract of Aconitum carmichaelii and the water extract of Citrus chinensis peel is 8:3:3; in step (3), the weight ratio of the liposome loaded with the antibacterial substance to the modified sodium hyaluronate solution is 1:

9.

10. A skin repair and whitening dressing based on an extract of black-skinned fir, characterized in that: The dressing is prepared by the preparation method according to any one of claims 1 to 9.

Citation Information

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