CN113662897A - Mouthwash and preparation method thereof - Google Patents

Mouthwash and preparation method thereof Download PDF

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Publication number
CN113662897A
CN113662897A CN202111171159.6A CN202111171159A CN113662897A CN 113662897 A CN113662897 A CN 113662897A CN 202111171159 A CN202111171159 A CN 202111171159A CN 113662897 A CN113662897 A CN 113662897A
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mouthwash
extract
parts
antibacterial peptide
honeysuckle
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CN113662897B (en
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徐德锋
陈秀竹
胡航
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Lichuan Changda Industrial Technology Research Institute Co ltd
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Lichuan Changda Industrial Technology Research Institute Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K36/18Magnoliophyta (angiosperms)
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    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484Glycyrrhiza (licorice)
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    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/71Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
    • A61K36/718Coptis (goldthread)
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K38/00Medicinal preparations containing peptides
    • A61K38/16Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
    • A61K38/17Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
    • A61K38/1703Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates
    • A61K38/1709Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates from mammals
    • A61K38/1729Cationic antimicrobial peptides, e.g. defensins
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
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    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/732Starch; Amylose; Amylopectin; Derivatives thereof
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    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5021Organic macromolecular compounds
    • A61K9/5036Polysaccharides, e.g. gums, alginate; Cyclodextrin
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    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04Antibacterial agents
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    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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Abstract

The invention discloses mouthwash, which comprises the following raw materials in parts by weight: 4-10 parts of coptis chinensis extract, 1-3 parts of honeysuckle extract, 0.5-2 parts of licorice extract, 1-2 parts of antibacterial peptide microcapsule, 0.6-1.2 parts of silk fibroin nanofiber, 1-2 parts of nonionic surfactant, 0.5-1 part of acidity regulator, 0.2-0.5 part of plant essence, 0.2-0.5 part of sweetening agent and 10-20 parts of ultrapure water; the mouthwash disclosed by the invention can clean dirt on the surfaces of teeth and gum, keep fresh breath and oral health, enable traditional Chinese medicine active molecules in coptis chinensis, honeysuckle and liquorice to be attached to antibacterial peptide to form a broad-spectrum antibacterial system, improve the killing effect on bacteria in the oral cavity, enable silk fibroin nanofibers to adjust the microbial environment of the oral cavity, effectively improve tooth sensitivity and reduce the incidence rate of caries, and is free of alcohol and high in safety.

Description

Mouthwash and preparation method thereof
Technical Field
The invention relates to the technical field of mouthwash, in particular to mouthwash and a preparation method thereof.
Background
Teeth are a portal of the oral cavity, and it is one of the health signs to have a healthy and white good teeth. Along with the improvement of living standard, the consciousness of people on oral health care is also greatly enhanced. The data show that the conventional tooth brushing can only remove 40-50% of dental plaque on the tooth surface, the dental plaque removing effect on oral soft tissues is basically ineffective, and for common oral diseases such as dental caries, oral ulcer and the like, a large amount of antibiotic medicines are used during treatment, so that the oral flora is unbalanced. The mouthwash as an oral care product can go deep into all parts of the oral cavity to assist in controlling bacterial plaque. At present, most of the available mouthwash uses essential oil or chlorhexidine as a bactericide, although the mouthwash containing the essential oil has strong permeability, the mouthwash contains alcohol and has an irritation effect on the oral cavity, and the mouthwash containing the chlorhexidine can form tartar after being used for a long time, so that the tooth surface is colored and the taste is changed.
Disclosure of Invention
In view of the above, the present invention provides a mouthwash and a preparation method thereof to solve the above problems.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the mouthwash comprises the following components in parts by weight: 4-10 parts of coptis chinensis extract, 1-3 parts of honeysuckle extract, 0.5-2 parts of licorice extract, 1-2 parts of antibacterial peptide microcapsule, 0.6-1.2 parts of silk fibroin nanofiber, 1-2 parts of nonionic surfactant, 0.5-1 part of acidity regulator, 0.2-0.5 part of plant essence, 0.2-0.5 part of sweetening agent and 20-30 parts of ultrapure water.
Further, the particle size of the antibacterial peptide microcapsule is 10-20 microns, and the antibacterial peptide is cationic antibacterial peptide.
Further, the diameter of the silk fibroin nanofiber is 1-100 nm.
Further, the nonionic surfactant is at least one of polyethylene glycol, polypropylene glycol, oleic acid polyoxyethylene ester, octyl phenol polyoxyethylene ether and styryl phenol polyoxyethylene ether.
Further, the acidity regulator is at least one of citric acid, malic acid, tartaric acid, acetic acid, lactic acid, fumaric acid, sodium citrate, potassium citrate and sodium acetate.
Further, the sweetener is at least one of xylitol, stevioside, aspartame, maltitol, sorbitol and erythritol.
Further, the plant essence is at least one of mint, jasmine, rose, sweet osmanthus, spearmint and orange.
Further, the preparation method of the mouthwash comprises the following steps:
(1) crushing coptis, adding the crushed coptis into water, adding absolute ethyl alcohol, uniformly stirring, heating and refluxing for extraction for 4-8 hours, and filtering and concentrating to obtain a coptis extract for later use;
(2) pulverizing honeysuckle, adding the pulverized honeysuckle into water, soaking for 18-24 hours at room temperature, filtering and concentrating to obtain a honeysuckle extract for later use;
(3) crushing liquorice, adding the crushed liquorice into water, soaking the liquorice for 18 to 24 hours at room temperature, filtering and concentrating to obtain a liquorice extract for later use;
(4) adding amylopectin into excessive water, heating and stirring uniformly in a constant-temperature water bath at 40-60 ℃ to obtain starch slurry, adding antibacterial peptide powder into the starch slurry, continuing to keep the temperature and stir for 1-2 hours to obtain starch antibacterial peptide slurry, cooling the starch antibacterial peptide slurry to room temperature, then performing centrifugal separation, taking a lower-layer solid, washing with deionized water for 3-5 times, and drying to obtain an antibacterial peptide microcapsule for later use;
(5) adding a formula amount of coptis chinensis extract, a honeysuckle extract, a liquorice extract, an antibacterial peptide microcapsule and silk fibroin nanofiber into ultrapure water, stirring and mixing at the room temperature at the rotating speed of 400-800 r/min for 20-40 min to obtain a mixture, sequentially adding a formula amount of a nonionic surfactant, a plant essence and a sweetening agent into the mixture, heating to 80-100 ℃, stirring at the rotating speed of 400-800 r/min for 1-2 h, adding an acidity regulator to adjust the pH value to 5.5-7, continuously stirring for 1-2 h, and cooling to obtain a mouthwash crude product;
(6) standing the crude product of the mouthwash overnight, filtering, sterilizing the filtrate by a pasteurization method, detecting, and filling to obtain the mouthwash.
Further, the mass ratio of the coptis chinensis to the absolute ethyl alcohol in the step (1) is 1-2: 1.
Further, the mass ratio of the antibacterial peptide powder to the amylopectin in the step (1) is 0.4-0.8: 1.
The mouthwash and the preparation method thereof have the beneficial effects that
(1) The invention takes the coptis extract, the honeysuckle extract, the liquorice extract and the antibacterial peptide as bactericides to prepare the mouthwash, and the coptis is a broad-spectrum antibacterial Chinese herbal medicine and has strong antibacterial property; the honeysuckle has the functions of resisting bacteria and viruses, diminishing inflammation and regulating immunity, the honeysuckle extract is matched with the coptis extract to inhibit various oral pathogenic bacteria such as staphylococcus aureus, escherichia coli, streptococcus mutans and the like, and meanwhile, the honeysuckle extract can promote the healing of the wound surface of the oral cavity; the liquorice is a tonifying Chinese herbal medicine, has a strong inhibiting effect on streptococcus mutans, can enhance the anti-caries capability of in-vitro teeth, and reduces the incidence rate of caries; the antibacterial peptide is used as a first defense line of innate immunity, has broad-spectrum antibacterial activity, can kill bacteria, fungi and viruses, is not easy to generate drug resistance, can promote angiogenesis, release histamine to cause vasodilatation, repair wounds and adjust the immune function of organisms under normal physiological conditions, has positive charges, can adsorb sterilization active molecules in the coptis chinensis extract, the honeysuckle extract and the liquorice extract to the periphery of the antibacterial peptide through electrostatic force to form a broad-spectrum antibacterial system, can puncture the cell wall of bacteria through electrostatic action to ensure that the sterilization active molecules in the coptis chinensis extract, the honeysuckle extract and the liquorice extract penetrate into the cell wall of the bacteria to kill the bacteria, thereby improving the sterilization effect, and meanwhile, the antibacterial peptide carrying the honeysuckle and the liquorice active molecules is attached to the epidermis and the teeth of the oral cavity, promoting the healing of the wound surface of the oral cavity, enhancing the anti-caries capability of the teeth and reducing the generation of dental caries.
(2) The added antibacterial peptide is dispersed in the mouthwash in a microcapsule form, the mouthwash is weakly acidic, and the cationic antibacterial peptide is alkaline, so that the antibacterial peptide has a good sterilization effect, the antibacterial peptide is coated by amylopectin which is insoluble in water as a wall material, the acidic mouthwash can promote saliva secretion of the oral cavity, the saliva is firstly reacted with acid in the mouthwash due to the fact that the pH of the saliva is about 7.2 and is weakly alkaline, and after the reaction, salivary amylase in the saliva carries out enzymolysis on the amylopectin into polysaccharide to slowly release the antibacterial peptide inside, so that the sterilization effect of the antibacterial peptide is guaranteed.
(3) The silk fibroin nanofiber is added to serve as a carrier of antibacterial peptide, amino acid of the silk fibroin mainly comprises glycine, alanine and serine, the amino acid is very close to horny rane of human hair and skin, the silk fibroin has excellent histocompatibility, adjustability and plasticity, cell adhesion can be promoted, the antibacterial peptide can be effectively adhered to the epidermis of an oral cavity through the silk fibroin nanofiber, and meanwhile, the silk fibroin carrying the antibacterial peptide can inhibit bacterial proliferation, relieve inflammation of the wound and promote wound healing, so that oral mucosa can be effectively repaired, and oral diseases are reduced.
Detailed Description
For further understanding of the present invention, the following detailed description is given in conjunction with specific examples, and the scope of the present invention is not limited thereto.
The invention provides mouthwash for cleaning oral cavity, which comprises the following components in parts by weight:
4-10 parts of coptis chinensis extract, 1-3 parts of honeysuckle extract, 0.5-2 parts of licorice extract, 1-2 parts of antibacterial peptide microcapsule, 0.6-1.2 parts of silk fibroin nanofiber, 1-2 parts of nonionic surfactant, 0.5-1 part of acidity regulator, 0.2-0.5 part of plant essence, 0.2-0.5 part of sweetening agent and 10-20 parts of ultrapure water; the antibacterial peptide is a cationic antibacterial peptide; the nonionic surfactant is at least one of polyethylene glycol, polypropylene glycol, oleic acid polyoxyethylene ester, octyl phenol polyoxyethylene ether and styryl phenol polyoxyethylene ether; the acidity regulator is at least one of citric acid, malic acid, tartaric acid, acetic acid, lactic acid, fumaric acid, sodium citrate, potassium citrate and sodium acetate; the sweetener is at least one of xylitol, stevioside, aspartame, maltitol, sorbitol and erythritol; the plant essence is at least one of herba Menthae, flos Jasmini sambac, flos Rosae Rugosae, flos Osmanthi Fragrantis, herba Menthae Rotundifoliae, and Mandarin orange.
The preparation method of the mouthwash comprises the following steps:
(1) weighing a certain amount of coptis chinensis and absolute ethyl alcohol according to the mass ratio of 1-2: 1, crushing the coptis chinensis, adding the crushed coptis chinensis into water, adding the absolute ethyl alcohol, uniformly stirring, heating and refluxing for extraction for 4-8 hours, filtering and concentrating to obtain a coptis chinensis extract for later use.
(2) Pulverizing honeysuckle, adding the pulverized honeysuckle into water, soaking for 18-24 hours at room temperature, filtering and concentrating to obtain a honeysuckle extract for later use.
(3) Crushing liquorice, adding the crushed liquorice into water, soaking the liquorice for 18 to 24 hours at room temperature, filtering and concentrating to obtain a liquorice extract for later use.
(4) Weighing a certain amount of antibacterial peptide powder and pullulan according to a mass ratio of 0.4-0.8: 1, adding the pullulan into excessive water, heating and stirring uniformly in a constant-temperature water bath at 40-60 ℃ to obtain starch slurry, adding the antibacterial peptide powder into the starch slurry, continuing to keep the temperature and stirring for 1-2 hours to obtain starch antibacterial peptide slurry, cooling the starch antibacterial peptide slurry to room temperature, then centrifugally separating, taking down the solid layer, washing with deionized water for 3-5 times, and drying to obtain the antibacterial peptide microcapsule for later use.
(5) Adding the coptis chinensis extract, the honeysuckle extract, the licorice extract, the antibacterial peptide microcapsule and the silk fibroin nanofiber into ultrapure water according to the formula amount, stirring and mixing at the room temperature at the rotating speed of 400-800 r/min for 20-40 min to obtain a mixture, sequentially adding the nonionic surfactant, the plant essence and the sweetening agent according to the formula amount into the mixture, heating to 80-100 ℃, stirring at the rotating speed of 400-800 r/min for 1-2 h, adding the acidity regulator to adjust the pH value to 5.5-7, continuously stirring for 1-2 h, and cooling to obtain a mouthwash crude product.
(6) Standing the crude product of the mouthwash overnight, filtering, sterilizing the filtrate by a pasteurization method, detecting, and filling to obtain the mouthwash.
Example 1
The mouthwash of this example comprises the following components:
4 parts of coptis chinensis extract, 1 part of honeysuckle extract, 0.5 part of liquorice extract, 1 part of antibacterial peptide microcapsule, 0.6 part of silk fibroin nanofiber, 1 part of polyethylene glycol, 0.5 part of citric acid, 0.2 part of mint essence, 0.2 part of xylitol and 10 parts of ultrapure water.
The preparation method of the mouthwash comprises the following steps:
(1) weighing a certain amount of coptis chinensis and absolute ethyl alcohol according to the mass ratio of 1:1, crushing the coptis chinensis, adding the crushed coptis chinensis into water, adding the absolute ethyl alcohol, uniformly stirring, heating and refluxing for extraction for 4 hours, and filtering and concentrating to obtain a coptis chinensis extract for later use.
(2) Pulverizing flos Lonicerae, adding into water, soaking at room temperature for 18 hr, filtering, and concentrating to obtain flos Lonicerae extract.
(3) Pulverizing Glycyrrhrizae radix, adding into water, soaking at room temperature for 18 hr, filtering, and concentrating to obtain Glycyrrhrizae radix extract.
(4) Weighing a certain amount of antibacterial peptide powder and pullulan according to the mass ratio of 0.4:1, adding the pullulan into excessive water, heating and stirring uniformly in a constant-temperature water bath at 40 ℃ to obtain starch slurry, adding the antibacterial peptide powder into the starch slurry, continuously keeping the temperature and stirring for 1h to obtain the starch antibacterial peptide slurry, cooling the starch antibacterial peptide slurry to room temperature, carrying out centrifugal separation, taking the lower-layer solid, washing with deionized water for 3 times, and drying to obtain the antibacterial peptide microcapsule for later use.
(5) Adding the coptis chinensis extract, the honeysuckle extract, the liquorice extract, the antibacterial peptide microcapsule and the silk fibroin nanofiber into ultrapure water according to the formula amount, stirring and mixing at the rotating speed of 400r/min for 20min at room temperature to obtain a mixture, sequentially adding the nonionic surfactant, the plant essence and the sweetening agent according to the formula amount into the mixture, heating to 80 ℃, stirring at the rotating speed of 400r/min for 1h, adding the acidity regulator to adjust the pH value to 5.5, continuously stirring for 1h, and cooling to obtain a mouthwash crude product.
(6) Standing the crude product of the mouthwash overnight, filtering, sterilizing the filtrate by a pasteurization method, detecting, and filling to obtain the mouthwash.
Example 2
The mouthwash and the preparation method thereof comprise the following steps:
7 parts of coptis chinensis extract, 2 parts of honeysuckle extract, 1 part of liquorice extract, 1.5 parts of antibacterial peptide microcapsule, 0.9 part of silk fibroin nanofiber, 1.5 parts of polypropylene glycol, 0.7 part of malic acid, 0.4 part of jasmine essence, 0.4 part of stevioside and 15 parts of ultrapure water.
The preparation method of the mouthwash comprises the following steps:
(1) weighing a certain amount of coptis chinensis and absolute ethyl alcohol according to the mass ratio of 1.5:1, crushing the coptis chinensis, adding the crushed coptis chinensis into water, adding the absolute ethyl alcohol, uniformly stirring, heating and refluxing for extraction for 6 hours, filtering and concentrating to obtain a coptis chinensis extract for later use.
(2) Pulverizing flos Lonicerae, adding into water, soaking at room temperature for 21 hr, filtering, and concentrating to obtain flos Lonicerae extract.
(3) Pulverizing Glycyrrhrizae radix, adding into water, soaking at room temperature for 21 hr, filtering, and concentrating to obtain Glycyrrhrizae radix extract.
(4) Weighing a certain amount of antibacterial peptide powder and pullulan according to the mass ratio of 0.6:1, adding the pullulan into excessive water, heating and stirring uniformly in a constant-temperature water bath at 50 ℃ to obtain starch slurry, adding the antibacterial peptide powder into the starch slurry, continuously keeping the temperature and stirring for 1.5 hours to obtain the starch antibacterial peptide slurry, cooling the starch antibacterial peptide slurry to room temperature, then centrifugally separating, taking the lower-layer solid, washing with deionized water for 4 times, and drying to obtain the antibacterial peptide microcapsule for later use.
(5) Adding the coptis chinensis extract, the honeysuckle extract, the liquorice extract, the antibacterial peptide microcapsule and the silk fibroin nanofiber into ultrapure water according to the formula amount, stirring and mixing at the room temperature at the rotating speed of 600r/min for 30min to obtain a mixture, sequentially adding the nonionic surfactant, the plant essence and the sweetening agent according to the formula amount into the mixture, heating to 90 ℃, stirring at the rotating speed of 600r/min for 1.5h, adding the acidity regulator to adjust the pH value to 6, continuously stirring for 1.5h, and cooling to obtain a mouthwash crude product.
(6) Standing the crude product of the mouthwash overnight, filtering, sterilizing the filtrate by a pasteurization method, detecting, and filling to obtain the mouthwash.
Example 3
The mouthwash and the preparation method thereof comprise the following steps:
10 parts of coptis extract, 3 parts of honeysuckle extract, 2 parts of liquorice extract, 2 parts of antibacterial peptide microcapsule, 1.2 parts of silk fibroin nanofiber, 2 parts of polyoxyethylene oleate, 1 part of tartaric acid, 0.5 part of rose essence, 0.5 part of aspartame and 20 parts of ultrapure water.
The preparation method of the mouthwash comprises the following steps:
(1) weighing a certain amount of coptis chinensis and absolute ethyl alcohol according to the mass ratio of 2:1, crushing the coptis chinensis, adding the crushed coptis chinensis into water, adding the absolute ethyl alcohol, uniformly stirring, heating and refluxing for extraction for 8 hours, and filtering and concentrating to obtain a coptis chinensis extract for later use.
(2) Pulverizing flos Lonicerae, adding into water, soaking at room temperature for 24 hr, filtering, and concentrating to obtain flos Lonicerae extract.
(3) Pulverizing Glycyrrhrizae radix, adding into water, soaking at room temperature for 24 hr, filtering, and concentrating to obtain Glycyrrhrizae radix extract.
(4) Weighing a certain amount of antibacterial peptide powder and pullulan according to a mass ratio of 0.8:1, adding the pullulan into excessive water, heating and stirring uniformly in a constant-temperature water bath at 60 ℃ to obtain starch slurry, adding the antibacterial peptide powder into the starch slurry, continuously keeping the temperature and stirring for 2 hours to obtain the starch antibacterial peptide slurry, cooling the starch antibacterial peptide slurry to room temperature, carrying out centrifugal separation, taking a lower-layer solid, washing with deionized water for 3-5 times, and drying to obtain the antibacterial peptide microcapsule for later use.
(5) Adding the coptis chinensis extract, the honeysuckle extract, the liquorice extract, the antibacterial peptide microcapsule and the silk fibroin nanofiber into ultrapure water according to the formula amount, stirring and mixing at the room temperature at the rotating speed of 800r/min for 40min to obtain a mixture, sequentially adding the nonionic surfactant, the plant essence and the sweetening agent according to the formula amount into the mixture, heating to 100 ℃, stirring at the rotating speed of 800r/min for 2h, adding the acidity regulator to adjust the pH value to 7, continuously stirring for 2h, and cooling to obtain a mouthwash crude product.
(6) Standing the crude product of the mouthwash overnight, filtering, sterilizing the filtrate by a pasteurization method, detecting, and filling to obtain the mouthwash.
Example 4
The mouthwash of this example is substantially the same as the mouthwash of example 1, except that the mouthwash of this example does not contain the antimicrobial peptide microcapsules and the silk fibroin nanofibers.
Example 5
The mouth rinse of this example is substantially the same as the mouth rinse of example 1, except that the mouth rinse of this example does not contain the coptis chinensis extract.
Experimental example 1
This example is an in vitro antibacterial test of the mouthwashes of examples 1 to 5
First, experiment principle
The antibacterial effect of the mouthwash of examples 1-5 on common strains is evaluated by using Minimum Inhibitory Concentration (MIC) and Minimum Bactericidal Concentration (MBC) indexes through in vitro antibacterial experiments.
Second, Experimental methods
Preparing bacterial liquid: selecting strains to inoculate in 20% cattle soaking juice culture medium, culturing overnight at 37 ℃, then diluting the bacteria liquid to 10cfu/mL by using the 20% cattle soaking juice culture medium, and immediately inoculating.
MIC determination: the sample was serially diluted in 20% bovine extract medium in a liquid tube serial dilution method. Adding 1.0mL into a sterilized test tube, adding 0.05mL of standard fresh bacterial liquid into each tube, setting a strain control group and a solvent control group, culturing at 37 ℃ for 18-24 hours, observing the growth condition of bacteria, and taking the highest dilution of aseptic growth as MIC.
MBC determination: the culture medium from two tubes evaluated as MIC and adjacent to MIC was inoculated to 10% serum MH broth agar by the plate streaking method, and cultured at 37 ℃ for 18-24 hours, with the highest dilution of no more than 5 growing colonies being MBC.
Third, test results
The test results are shown in Table 1.
Table 1: results of in vitro antibacterial test of mouth wash
Figure BDA0003293236940000091
Figure BDA0003293236940000101
As can be seen from table 1, the mouth wash prepared in examples 1 to 5 has different degrees of inhibition and killing effects on escherichia coli, staphylococcus aureus, escherichia coli, typhoid bacillus, mold, candida albicans and pseudomonas aeruginosa, and the killing effect on bacteria in examples 1 to 3 is significantly higher than that in examples 4 and 5, because the sterilization active molecules in the coptis chinensis extract, the honeysuckle extract and the licorice extract in examples 1 to 3 can be attached to the molecular chain of the antibacterial peptide to form a broad-spectrum antibacterial system, the coptis chinensis extract, the honeysuckle extract and the licorice extract firstly contact the oral cavity to kill bacteria, then the antibacterial peptide is attached to the epidermis and teeth of the oral cavity through silk fibroin fibers to kill bacteria continuously, so that the sterilization effect of the mouth wash is ensured, because example 4 does not contain antibacterial peptide microcapsules and silk fibroin nanofibers, although the coptis extract, the honeysuckle extract and the liquorice extract have the bactericidal effect, the synergistic effect with the antibacterial peptide is lacked, the bactericidal effect is slightly reduced compared with that of the embodiment 1-3, while the embodiment 5 does not contain the coptis extract, the coptis extract and the coptis as a broad-spectrum antibacterial Chinese herbal medicine have strong antibacterial property, and the bactericidal effect is obviously reduced due to the lack of the mouthwash of the coptis extract.
Experimental example 2
This example is a skin irritation test of the mouthwashes of examples 1 to 5
Toxicology experiments were performed on the mouthwashes of examples 1 to 5 according to the "cosmetic hygiene code" 2007 edition of the ministry of health, and the irritation of the mouthwashes of examples 1 to 5 on guinea pig skin was verified.
First, acute skin irritation experiment
40 guinea pigs were divided into 4 groups of 10 animals each, and both sides of the spine were cut off with a hair removal range of 3 × 3cm each, 0.5g of each of the mouthwashes of examples 1 to 5 was applied to one side of the skin of the guinea pigs of the corresponding group, covered with two layers of gauze and a layer of cellophane, and then fixed with a non-irritating adhesive tape, and the other side was used as a control. And (4) performing a sealing experiment, applying for 4h, and cleaning with warm water to remove residual test samples after 4 h.
The skin reaction of the applied part was observed for 1h, 24h, 48h, and 72h after the test sample was removed, and the skin reaction score was performed as shown in table 2.
Multiple skin irritation test
40 guinea pigs were divided into 4 groups of 10 animals each, and both sides of the spine were cut off with a hair removal range of 3 × 3cm each and an application area of 2.5cm × 2.5cm, and about 0.5g of mouthwash A, B, C, D was applied to one side of the skin and the other side as a control, once a day for 14 days, continuously, cut hair from day 2 before application, washed with water to remove residual test sample, and skin reactions were observed after 1h and scored according to table 2.
Table 2: skin irritation response score
Figure BDA0003293236940000111
According to the experimental method, the integral of the evaluation result of the mouthwash of embodiments 1 to 5 in the skin irritation experiment is 0, because the invention adopts the coptis chinensis extract, the honeysuckle extract, the licorice extract and the antimicrobial peptide as the bactericide, and the broad-spectrum bactericidal system formed by attaching the bactericidal active molecules in the coptis chinensis extract, the honeysuckle extract and the licorice extract to the antimicrobial peptide has high biocompatibility and no harm to cells, and meanwhile, the mouthwash does not contain irritant raw materials such as essential oil and alcohol, and has small irritation to the skin.
Experimental example 3
This experiment example is an experiment for improving gingival sensitivity with mouthwash of examples 1 to 5
100 volunteers with tooth sensitivity are randomly selected and divided into five groups, 20 persons in each group are treated by the mouthwash in the embodiment 1-5 for 3 times a day, the mouth cavity contains 1-2 min each time, and after 20 days, the tooth sensitivity improvement condition is counted, and the statistical result is shown in table 3.
Table 3: statistics of tooth sensitivity improvement
Example 1 Example 2 Example 3 Example 4 Example 5
Reduced number of people with sensitivity 17 19 18 13 15
Sensitivity reduction 18 19 20 12 16
As shown in table 3, the mouth wash of examples 1 to 3 was used to clean and care the oral cavity, since the fibroin nanofibers carried the antibacterial peptides and the herbal extracts attached to the surfaces of the teeth and gums, the amino acids of fibroin were mainly glycine, alanine and serine, which are very close to the horny raney of human hair and skin, and had excellent histocompatibility, adjustability and plasticity, and could promote the adhesion of cells, the antibacterial peptides could be effectively adhered to the epidermis of the oral cavity through the fibroin nanofibers, and at the same time, the fibroin carrying the antibacterial peptides could inhibit the proliferation of bacteria, alleviate the inflammation of the wound, and promote the healing of the wound, thereby effectively repairing the oral mucosa and improving the condition of tooth allergy.
(1) The invention takes the coptis extract, the honeysuckle extract, the liquorice extract and the antibacterial peptide as bactericides to prepare the mouthwash, and the coptis is a broad-spectrum antibacterial Chinese herbal medicine and has strong antibacterial property; the honeysuckle has the functions of resisting bacteria and viruses, diminishing inflammation and regulating immunity, the honeysuckle extract is matched with the coptis extract to inhibit various oral pathogenic bacteria such as staphylococcus aureus, escherichia coli, streptococcus mutans and the like, and meanwhile, the honeysuckle extract can promote the healing of the wound surface of the oral cavity; the liquorice is a tonifying Chinese herbal medicine, has a strong inhibiting effect on streptococcus mutans, can enhance the anti-caries capability of in-vitro teeth, and reduces the incidence rate of caries; the antibacterial peptide is used as a first defense line of innate immunity, has broad-spectrum antibacterial activity, can kill bacteria, fungi and viruses, is not easy to generate drug resistance, can promote angiogenesis, release histamine to cause vasodilatation, repair wounds and adjust the immune function of organisms under normal physiological conditions, has positive charges, can adsorb sterilization active molecules in the coptis chinensis extract, the honeysuckle extract and the liquorice extract to the periphery of the antibacterial peptide through electrostatic force to form a broad-spectrum antibacterial system, can puncture the cell wall of bacteria through electrostatic action to ensure that the sterilization active molecules in the coptis chinensis extract, the honeysuckle extract and the liquorice extract penetrate into the cell wall of the bacteria to kill the bacteria, thereby improving the sterilization effect, and meanwhile, the antibacterial peptide carrying the honeysuckle and the liquorice active molecules is attached to the epidermis and the teeth of the oral cavity, promoting the healing of the wound surface of the oral cavity, enhancing the anti-caries capability of the teeth and reducing the generation of dental caries.
Experimental example 4
This example is a breath freshening experiment for cleaning and maintaining the mouth rinse of examples 1-5
First, experimental scheme
40 volunteers were randomly located and divided into five groups of 8 individuals each for testing the mouthwash of the invention.
The testee firstly rinses mouth with clear water to remove food residues left in the oral cavity as much as possible; then, about 10mL of mouthwash is used for gargling for about 1min, and the gargling is finished without rinsing with clear water. The OD value of the bacteria in the oral cavity was measured every 2h by UV spectrophotometry.
Second, the experimental results are shown in table 4.
Table 4: experimental conditions of mouthwash of examples 1-5 on growth of flora
Time (h) Example 1 Example 2 Example 3 Example 4 Example 5
2 0.008 0.028 0.022 0.051 0.108
4 0.032 0.038 0.031 0.063 0.157
6 0.077 0.096 0.075 0.145 0.336
8 0.102 0.114 0.102 0.192 0.468
As can be seen from table 4, the mouth washes of examples 1 to 3 have good cleaning effects and can keep fresh breath for a long time of 8 hours, but the cleaning effects of examples 4 and 5 are general and the maintenance time is short. The reason is that in the mouthwash of examples 1 to 3, the antibacterial peptide with positive charges can adsorb the sterilization active molecules in the coptis chinensis extract, the honeysuckle extract and the liquorice extract to the surroundings through electrostatic force to form a broad-spectrum antibacterial system, the antibacterial peptide can puncture the cell walls of bacteria through the electrostatic action, so that the sterilization active molecules in the coptis chinensis extract, the honeysuckle extract and the liquorice extract penetrate into the cell walls of the bacteria to kill the bacteria, meanwhile, the antibacterial peptide can be attached to the oral cavity epidermis and the teeth for a long time through the silk fibroin nano-fiber, the sterilization effect of the mouthwash is improved, since example 4 does not contain the antimicrobial peptide microcapsules and the silk fibroin nanofibers, the duration of sterilization is short, the coptis extract is absent in example 5, and the sterilization effect is low, so that neither the mouth rinses of example 4 nor example 5 can inhibit the proliferation of flora in the oral cavity for a long time.
Therefore, the mouthwash of the invention has large killing effect on bacteria in the oral cavity and long duration, can adjust the microbial environment of the oral cavity, effectively improve the tooth sensitivity and reduce the incidence rate of caries, and is free of alcohol and high in safety.
Various other modifications and changes may be made by those skilled in the art based on the above-described technical solutions and concepts, and all such modifications and changes should fall within the scope of the claims of the present invention.

Claims (10)

1. The mouthwash is characterized by comprising the following components in parts by weight: 4-10 parts of coptis chinensis extract, 1-3 parts of honeysuckle extract, 0.5-2 parts of licorice extract, 1-2 parts of antibacterial peptide microcapsule, 0.6-1.2 parts of silk fibroin nanofiber, 1-2 parts of nonionic surfactant, 0.5-1 part of acidity regulator, 0.2-0.5 part of plant essence, 0.2-0.5 part of sweetening agent and 20-30 parts of ultrapure water.
2. The mouthwash according to claim 1, wherein the antibacterial peptide microcapsules have a particle size of 10-20 μm, and the antibacterial peptide is a cationic antibacterial peptide.
3. The mouthwash of claim 1, wherein the silk fibroin nanofibers have a diameter of 1-100 nm.
4. The mouthwash of claim 1, wherein the nonionic surfactant is at least one of polyethylene glycol, polypropylene glycol, polyoxyethylene oleate, polyoxyethylene octylphenol ether, and polyoxyethylene styrylphenol ether.
5. The mouthwash of claim 1, wherein the acidity regulator is at least one of citric acid, malic acid, tartaric acid, acetic acid, lactic acid, fumaric acid, sodium citrate, potassium citrate, and sodium acetate.
6. The mouthwash of claim 1, wherein the sweetener is at least one of xylitol, stevioside, aspartame, maltitol, sorbitol, erythritol.
7. The mouthwash according to claim 1, wherein the plant flavor is at least one of mint, jasmine, rose, sweet osmanthus, spearmint, and citrus.
8. A preparation method of mouthwash is characterized by comprising the following steps:
(1) crushing coptis, adding the crushed coptis into water, adding absolute ethyl alcohol, uniformly stirring, heating and refluxing for extraction for 4-8 hours, and filtering and concentrating to obtain a coptis extract for later use;
(2) pulverizing honeysuckle, adding the pulverized honeysuckle into water, soaking for 18-24 hours at room temperature, filtering and concentrating to obtain a honeysuckle extract for later use;
(3) crushing liquorice, adding the crushed liquorice into water, soaking the liquorice for 18 to 24 hours at room temperature, filtering and concentrating to obtain a liquorice extract for later use;
(4) adding amylopectin into excessive water, heating and stirring uniformly in a constant-temperature water bath at 40-60 ℃ to obtain starch slurry, adding antibacterial peptide powder into the starch slurry, continuing to keep the temperature and stir for 1-2 hours to obtain starch antibacterial peptide slurry, cooling the starch antibacterial peptide slurry to room temperature, then performing centrifugal separation, taking a lower-layer solid, washing with deionized water for 3-5 times, and drying to obtain an antibacterial peptide microcapsule for later use;
(5) adding a formula amount of coptis chinensis extract, a honeysuckle extract, a liquorice extract, an antibacterial peptide microcapsule and silk fibroin nanofiber into ultrapure water, stirring and mixing at the room temperature at the rotating speed of 400-800 r/min for 20-40 min to obtain a mixture, sequentially adding a formula amount of a nonionic surfactant, a plant essence and a sweetening agent into the mixture, heating to 80-100 ℃, stirring at the rotating speed of 400-800 r/min for 1-2 h, adding an acidity regulator to adjust the pH value to 5.5-7, continuously stirring for 1-2 h, and cooling to obtain a mouthwash crude product;
(6) standing the crude product of the mouthwash overnight, filtering, sterilizing the filtrate by a pasteurization method, detecting, and filling to obtain the mouthwash.
9. The preparation method of the mouthwash according to claim 8, wherein the mass ratio of the coptis chinensis to the absolute ethyl alcohol in the step (1) is 1-2: 1.
10. The preparation method of mouthwash according to claim 8, wherein the mass ratio of the antibacterial peptide powder to the amylopectin in step (4) is 0.4-0.8: 1.
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