CN109528601B - Compound traditional Chinese medicine mouth wash and preparation method thereof - Google Patents

Compound traditional Chinese medicine mouth wash and preparation method thereof Download PDF

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CN109528601B
CN109528601B CN201910054886.0A CN201910054886A CN109528601B CN 109528601 B CN109528601 B CN 109528601B CN 201910054886 A CN201910054886 A CN 201910054886A CN 109528601 B CN109528601 B CN 109528601B
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chinese medicine
traditional chinese
extract
water
parts
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CN109528601A (en
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谷筱玉
缪剑华
刘凡
王硕
龚小妹
欧春丽
莫单丹
马庆峰
周小雷
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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
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18

Abstract

The invention discloses a compound traditional Chinese medicine mouthwash which comprises the following raw materials in parts by weight: 12-15% of traditional Chinese medicine composition extract, 0.01-1% of sweetening agent, 0.02-1% of sour agent, 2-10% of humectant, 0.01-0.4% of preservative, 0.5-5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 20-23 parts of agastache rugosus, 12-15 parts of lonicera confusa and 2-3 parts of pseudo-ginseng. The invention also discloses a preparation method of the compound traditional Chinese medicine mouthwash. The oral liquid has the beneficial effects of diminishing inflammation, inhibiting bacteria, effectively removing food residues and soft dirt remained in the oral cavity and simultaneously quickly relieving the gingival pain.

Description

Compound traditional Chinese medicine mouth wash and preparation method thereof
Technical Field
The invention relates to the field of mouthwash preparation. More specifically, the invention relates to a compound traditional Chinese medicine mouthwash and a preparation method thereof.
Background
Along with the development of society, the contents of life, work and activities of people are increased, people want to carry out various activities needing language communication such as social contact, negotiation, report, work, entertainment, emotion communication and the like all day long, if people have halitosis or smoke, drink wine and eat peculiar smell food, people can solve the problem by gargling with clear water, the problem is not solved, chewing gum is not elegant (particularly for middle-aged and old people), and people can not bring the special chewing gum with the teeth; the mouthwash is taken as an oral health product, and is popular with people due to the characteristics of simplicity, convenience, cleanness and sanitation.
At present, a lot of traditional Chinese medicines related to mouthwash have the effects of removing oral residues and freshening breath, but the basic of daily oral health care lies in preventing and controlling oral diseases related to dental plaque, such as gingivitis, periodontitis and the like, wherein the gum is one of periodontal tissues and is directly exposed in the oral cavity, harmful substances in dental plaque machines accumulated at the junction of the gum and the teeth act on the gum for a long time to cause inflammation, and the existence of tartar, bad restorations, food impaction, crowding of teeth, mouth breathing and the like aggravates the accumulation of dental plaque and the inflammation of the gum, and bacteriostasis or sterilization by using an effective chemical preparation is an effective way for controlling the dental plaque, and the conventional chemical preparation can cause potential risks of drug resistance, and oral cavity pain caused by gingivitis and periodontitis can cause extreme discomfort of patients.
In view of the above situation, it is an urgent need to solve the problem of providing a mouthwash which has antibacterial and bactericidal effects on common oral bacteria and effectively relieves gum pain.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
Still another object of the present invention is to provide a compound Chinese medicinal mouthwash which is capable of diminishing inflammation, inhibiting bacteria, effectively removing food residues and soft dirt remaining in the oral cavity, and simultaneously rapidly relieving gum pain.
The invention also aims to provide a preparation method of the compound traditional Chinese medicine mouthwash, which is obtained by multiple times of water boiling and alcohol precipitation and has the effects of diminishing inflammation and inhibiting bacteria.
In order to achieve these objects and other advantages in accordance with the present invention, there is provided a compound Chinese medicinal mouthwash comprising the following raw materials in parts by weight:
12-15% of traditional Chinese medicine composition extract, 0.01-1% of sweetening agent, 0.02-1% of sour agent, 2-10% of humectant, 0.01-0.4% of preservative, 0.5-5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 20-23 parts of agastache rugosus, 12-15 parts of lonicera confusa and 2-3 parts of pseudo-ginseng.
Preferably, the raw material medicines of the traditional Chinese medicine extract also comprise: 7-8 parts of pepper and 2-5 parts of eupatorium.
Preferably, the sweetening agent is one or more of sucralose, fructose and stevioside, the sour agent is one of malic acid, citric acid and tartaric acid, the humectant is one of glycerin and sorbitol, and the preservative is one or more of methyl paraben, ethyl paraben and sodium benzoate.
A preparation method of a living compound traditional Chinese medicine mouthwash comprises the following steps:
the method comprises the following steps:
s1, weighing herba Agastaches, flos Lonicerae, and radix Notoginseng in proportion, mixing to obtain a Chinese medicinal mixture, adding 15 times of water into the Chinese medicinal mixture, boiling and extracting for 2 times, 2 hr for the first time, 1.5 hr for the second time, mixing the filtrates obtained by 2 times of extraction, concentrating under reduced pressure to obtain a concentrated solution, adding ethanol into the concentrated solution to make the alcohol content reach 60%, stirring, mixing, standing for 24 hr, filtering to remove precipitate to obtain an ethanol precipitation filtrate, and concentrating the ethanol precipitation filtrate to obtain a Chinese medicinal extract;
s2, mixing the Chinese medicinal extract, sweetener, sour agent, humectant, antiseptic, menthol and water, and packaging.
Preferably, the specific gravity of the concentrated solution in the step S1 is 1.02-1.10 at 80 ℃, and the specific gravity of the Chinese medicinal composition extract is 1.06-1.12 at 80 ℃.
Preferably, the agastache rugosa is fresh agastache rugosa leaves, and the fresh agastache rugosa leaves are equally divided into three parts in step S1;
one part of fresh agastache rugosus leaves are dried in a 65 ℃ oven to constant weight after being dried in the sun and nightly for 3-4 days continuously, ground into powder and sieved by a 200-mesh sieve at 100 ℃, so as to obtain agastache rugosus powder, water with the amount of 8 times of the total mass of the powder is added into the powder, and the powder is soaked for 5 hours and then subjected to steam distillation extraction for 4 hours, so as to obtain agastache rugosus essential oil;
adding 0.05 times of lemon juice and 1 time of water into the other part of fresh agastache rugosus leaf, pulping to obtain a pulp, cooling the pulp to-20 ℃, keeping the temperature for 3 hours, taking out the pulp, thawing at room temperature to obtain a frozen pulp, adding 2 times of water into the frozen pulp, filtering to obtain a first filtrate and a first filter residue, adding 4 times of water into the first filtrate, stirring for 10 minutes, filtering to obtain a second filtrate, combining the first filtrate and the second filtrate, and concentrating to obtain a first extract;
sun drying the last fresh folium Agastaches until the water content is less than 12% to obtain dry folium Agastaches, and mixing dry folium Agastaches, flos Lonicerae and Notoginseng radix to obtain Chinese medicinal mixture;
step S2 is to mix the Chinese medicinal extract, herba Agastaches essential oil, extract, sweetener, sour agent, humectant, antiseptic, menthol and water thoroughly, and subpackage.
Preferably, step S1 further includes:
weighing 7-8 parts of pepper, grinding into powder, adding water with the amount being 10 times of the total mass of the pepper, boiling and extracting for 2 times, 2 hours for the first time and 1 hour for the second time, combining filtrate obtained by 2 times of extraction, and concentrating to obtain a second extract;
weighing 2-5 parts of eupatorium fortunei, grinding into powder, adding water with the amount being 10 times of the total mass of the eupatorium fortunei, boiling and extracting for 2 times, the first time for 3 hours and the second time for 2 hours, combining filter liquor extracted for 2 times, concentrating to obtain a third extract, adding water to dilute the third extract, then carrying out alcohol precipitation, stirring and uniformly mixing, standing for 2 hours, filtering to obtain a first alcohol precipitate, adding water to dissolve the first alcohol precipitate, then carrying out alcohol precipitation, stirring and uniformly mixing, standing for 2 hours, and filtering to obtain a second alcohol precipitate;
step S2 is to mix the Chinese medicinal extract, herba Agastaches essential oil, first extract, second alcohol precipitate, sweetener, sour agent, humectant, antiseptic, menthol and water thoroughly, and subpackage.
The invention at least comprises the following beneficial effects:
firstly, the traditional Chinese medicine components including the extracts of wrinkled gianthyssop herb, lonicera confusa and pseudo-ginseng are added into the mouthwash, so that dental plaque can be effectively inhibited, peculiar smell in the oral cavity can be removed, periodontitis and gingivitis can be prevented, oral pain caused by periodontitis and gingivitis can be effectively relieved, and the mouthwash has good effects of cleaning and nursing the oral cavity;
secondly, the traditional Chinese medicine formula contained in the mouthwash is simple, the raw materials are easy to obtain, the cost is low, the traditional Chinese medicine mixture is subjected to twice water boiling and once alcohol precipitation to obtain the traditional Chinese medicine composite extract, the preparation method is simple, the process is stable, and the large-scale production can be realized;
thirdly, respectively carrying out dry-leaf steam distillation on fresh agastache rugosus leaves to obtain agastache rugosus essential oil, pulping the fresh leaves, then carrying out freezing extraction to obtain a first extract, and carrying out water boiling and alcohol precipitation on the panax notoginseng and the lonicera confusa to obtain a traditional Chinese medicine combined extract, so that the extraction amount of agastache rugosus ketone, cinnamaldehyde and other components with good antifungal effects in the agastache rugosus can be effectively increased, the antibacterial effect of the mouthwash is improved, and meanwhile, the agastache rugosus essential oil in the mouthwash can be volatilized a small amount to enter a human body through an oral cavity during use, so that the mouthwash has the effects of stimulating gastrointestinal secretion, improving the activity of pepsin, promoting fresh breath and relieving; the addition of the pepper and the eupatorium, and the further combination of the agastache rugosus, the lonicera confusa and the pseudo-ginseng can effectively improve the effect of the mouthwash on relieving oral cavity pain caused by gingivitis and periodontitis.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
< example 1>
The compound traditional Chinese medicine mouthwash comprises the following raw materials in parts by weight:
12% of traditional Chinese medicine composition extract, 0.01% of sucralose, 0.02% of malic acid, 2% of glycerol, 0.01% of methyl paraben, 0.5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 20 parts of wrinkled gianthyssop herb, 12 parts of lonicera confusa and 2 parts of pseudo-ginseng.
The preparation method of the compound traditional Chinese medicine mouthwash comprises the following steps:
s1, weighing herba Agastaches, flos Lonicerae, and radix Notoginseng in proportion, mixing to obtain a Chinese medicinal mixture, adding 15 times of water into the Chinese medicinal mixture, boiling and extracting for 2 times, 2 hr for the first time, 1.5 hr for the second time, mixing the filtrates obtained by 2 times, concentrating under reduced pressure to obtain a concentrated solution (the specific gravity at 80 deg.C is 1.05), adding ethanol into the concentrated solution to make the ethanol content reach 60%, stirring, mixing, standing for 24 hr, filtering to remove precipitate to obtain an ethanol precipitation filtrate, and concentrating the ethanol precipitation filtrate to obtain a Chinese medicinal extract (the specific gravity at 80 deg.C is 1.07);
s2, mixing the above Chinese medicinal extracts, sucralose, malic acid, glycerol, methyl hydroxybenzoate, menthol and water, and packaging.
< example 2>
The compound traditional Chinese medicine mouthwash comprises the following raw materials in parts by weight:
13% of traditional Chinese medicine composition extract, 0.05% of fructose, 0.06% of citric acid, 6% of sorbitol, 0.28% of ethylparaben, 3.5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 22 parts of wrinkled gianthyssop herb, 13 parts of lonicera confusa and 2.5 parts of pseudo-ginseng.
The preparation method of the compound traditional Chinese medicine mouthwash comprises the following steps:
s1, weighing herba Agastaches, flos Lonicerae, and radix Notoginseng in proportion, mixing to obtain a Chinese medicinal mixture, adding 15 times of water into the Chinese medicinal mixture, boiling and extracting for 2 times, 2 hr for the first time, 1.5 hr for the second time, mixing the filtrates obtained by 2 times, concentrating under reduced pressure to obtain a concentrated solution (the specific gravity at 80 deg.C is 1.06), adding ethanol into the concentrated solution to make the ethanol content reach 60%, stirring, mixing, standing for 24 hr, filtering to remove precipitate to obtain an ethanol precipitation filtrate, and concentrating the ethanol precipitation filtrate to obtain a Chinese medicinal extract (the specific gravity at 80 deg.C is 1.08);
s2, mixing the above Chinese medicinal extracts, fructose, citric acid, sorbitol, ethylparaben, menthol and water, and packaging.
< example 3>
The compound traditional Chinese medicine mouthwash comprises the following raw materials in parts by weight:
15% of traditional Chinese medicine composition extract, 1% of stevioside, 1% of tartaric acid, 10% of sorbitol, 0.4% of sodium benzoate, 5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 23 parts of agastache rugosus, 15 parts of lonicera confusa and 3 parts of pseudo-ginseng.
The preparation method of the compound traditional Chinese medicine mouthwash comprises the following steps:
s1, weighing herba Agastaches, flos Lonicerae, and radix Notoginseng in proportion, mixing to obtain a Chinese medicinal mixture, adding 15 times of water into the Chinese medicinal mixture, boiling and extracting for 2 times, 2 hr for the first time, 1.5 hr for the second time, mixing the filtrates obtained by 2 times, concentrating under reduced pressure to obtain a concentrated solution (the specific gravity at 80 deg.C is 1.10), adding ethanol into the concentrated solution to make the ethanol content reach 60%, stirring, mixing, standing for 24 hr, filtering to remove precipitate to obtain an ethanol precipitation filtrate, and concentrating the ethanol precipitation filtrate to obtain a Chinese medicinal extract (the specific gravity at 80 deg.C is 1.10);
s2, mixing the Chinese medicinal extract, stevioside, tartaric acid, sorbitol, sodium benzoate, menthol and water, and packaging.
< example 4>
The compound traditional Chinese medicine mouthwash comprises the following raw materials in parts by weight:
13% of traditional Chinese medicine composition extract, 0.05% of fructose, 0.06% of citric acid, 6% of sorbitol, 0.28% of ethylparaben, 3.5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 22 parts of wrinkled gianthyssop herb, 13 parts of lonicera confusa and 2.5 parts of pseudo-ginseng.
The preparation method of the compound traditional Chinese medicine mouthwash comprises the following steps:
s1, dividing the fresh agastache rugosus leaves into three parts;
one part of fresh agastache rugosus leaves are dried in a 65 ℃ oven to constant weight after being dried in the sun and nightly for 3 days continuously, ground into powder and sieved by a 200-mesh sieve with 100 meshes, so as to obtain agastache rugosus powder, water with the amount of 8 times of the total mass of the powder is added into the powder, and after the powder is soaked for 5 hours, steam distillation extraction is carried out for 4 hours, so as to obtain agastache rugosus essential oil;
adding 0.05 times of lemon juice and 1 time of water into the other part of fresh agastache rugosus leaf, pulping to obtain a pulp, cooling the pulp to-20 ℃, keeping the temperature for 3 hours, taking out the pulp, thawing at room temperature to obtain a frozen pulp, adding 2 times of water into the frozen pulp, filtering to obtain a first filtrate and a first filter residue, adding 4 times of water into the first filtrate, stirring for 10 minutes, filtering to obtain a second filtrate, combining the first filtrate and the second filtrate, and concentrating to obtain a first extract;
sun-drying the last fresh patchouli leaf until the water content is 11.5% to obtain dry patchouli leaves, weighing the lonicera confusa and the pseudo-ginseng according to the proportion, mixing the dry patchouli leaves, the lonicera confusa and the pseudo-ginseng to obtain a traditional Chinese medicine mixture, adding water with the amount 15 times of the total mass of the traditional Chinese medicine mixture into the traditional Chinese medicine mixture, boiling and extracting for 2 times, 2 hours for the first time and 1.5 hours for the second time, combining the filtrate obtained by 2 times of extraction, concentrating under reduced pressure to obtain a concentrated solution (the specific gravity is 1.03 at 80 ℃), adding ethanol into the concentrated solution to ensure that the alcohol content is 60%, stirring, uniformly mixing, standing for 24 hours, filtering to remove precipitates to obtain an ethanol precipitation filtrate, and concentrating the ethanol precipitation filtrate to obtain;
s2, mixing the Chinese medicinal extract, herba Agastaches essential oil, the first extract, fructose, citric acid, sorbitol, ethylparaben, menthol and water, and packaging.
< example 5>
The compound traditional Chinese medicine mouthwash comprises the following raw materials in parts by weight:
13% of traditional Chinese medicine composition extract, 0.05% of fructose, 0.06% of citric acid, 6% of sorbitol, 0.28% of ethylparaben, 3.5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 22 parts of wrinkled gianthyssop herb, 13 parts of lonicera confusa and 2.5 parts of pseudo-ginseng.
The preparation method of the compound traditional Chinese medicine mouthwash comprises the following steps:
s1, dividing the fresh agastache rugosus leaves into three parts;
one part of fresh agastache rugosus leaves are dried in a 65 ℃ oven to constant weight after being dried in the sun and nightly for 3 days continuously, ground into powder and sieved by a 200-mesh sieve with 100 meshes, so as to obtain agastache rugosus powder, water with the amount of 8 times of the total mass of the powder is added into the powder, and after the powder is soaked for 5 hours, steam distillation extraction is carried out for 4 hours, so as to obtain agastache rugosus essential oil;
adding 0.05 times of lemon juice and 1 time of water into the other part of fresh agastache rugosus leaf, pulping to obtain a pulp, cooling the pulp to-20 ℃, keeping the temperature for 3 hours, taking out the pulp, thawing at room temperature to obtain a frozen pulp, adding 2 times of water into the frozen pulp, filtering to obtain a first filtrate and a first filter residue, adding 4 times of water into the first filtrate, stirring for 10 minutes, filtering to obtain a second filtrate, combining the first filtrate and the second filtrate, and concentrating to obtain a first extract;
sun-drying the last fresh patchouli leaf until the water content is 10.9% to obtain dry patchouli leaves, weighing the lonicera confusa and the pseudo-ginseng according to the proportion, mixing the dry patchouli leaves, the lonicera confusa and the pseudo-ginseng to obtain a traditional Chinese medicine mixture, adding water with the amount 15 times of the total mass of the traditional Chinese medicine mixture into the traditional Chinese medicine mixture, boiling and extracting for 2 times, 2 hours for the first time and 1.5 hours for the second time, combining the filtrate obtained by 2 times of extraction, concentrating under reduced pressure to obtain a concentrated solution (the specific gravity is 1.09 at 80 ℃), adding ethanol into the concentrated solution to ensure that the alcohol content is 60%, stirring, uniformly mixing, standing for 24 hours, filtering to remove precipitates to obtain an ethanol precipitation filtrate, and concentrating the ethanol precipitation filtrate to obtain;
weighing 7-8 parts of pepper, grinding into powder, adding water with the amount being 10 times of the total mass of the pepper, boiling and extracting for 2 times, 2 hours for the first time and 1 hour for the second time, combining filtrate obtained by 2 times of extraction, and concentrating to obtain a second extract;
weighing 2-5 parts of eupatorium fortunei, grinding into powder, adding water with the amount being 10 times of the total mass of the eupatorium fortunei, boiling and extracting for 2 times, the first time for 3 hours and the second time for 2 hours, combining filter liquor extracted for 2 times, concentrating to obtain a third extract, adding water to dilute the third extract, then carrying out alcohol precipitation, stirring and uniformly mixing, standing for 2 hours, filtering to obtain a first alcohol precipitate, adding water to dissolve the first alcohol precipitate, then carrying out alcohol precipitation, stirring and uniformly mixing, standing for 2 hours, and filtering to obtain a second alcohol precipitate;
s2, mixing the Chinese medicinal extract, herba Agastaches essential oil, the first extract, the second alcohol precipitate, fructose, citric acid, sorbitol, ethylparaben, menthol and water, and packaging.
Experiment of
1. Acute toxicity test
The preparation method comprises the steps of concentrating the solution prepared in the embodiment 5 to constant weight, dissolving the solution in water to prepare 0.5g/mL suspension, selecting 10 mice male and female respectively, performing irrigation, and performing irrigation feeding according to the dosage of 10g (bulk drug)/kg (weight of the mice), wherein after the irrigation feeding, no death and abnormality of the mice are observed for 72 hours, which indicates that the tolerance is large.
2. Antibacterial test (the bacteria used are all international standard strains)
2.1, bacterial species: staphylococcus aureus, Candida albicans, Streptococcus mutans, Lactobacillus, Porphyromonas gingivalis.
2.2 preparation of bacterial culture Medium
Solid medium: weighing 30g of trypticase soybean broth, adding 15g of basic agar, dissolving with 1000mL of purified water at 100 ℃, sterilizing for 20min by using high-pressure steam at 120 ℃ and 110kpa, cooling to 50-60 ℃, and preserving at constant temperature for later use;
liquid culture medium: weighing 6g of trypticase soybean broth, dissolving with 200mL of purified water at 100 ℃, sterilizing for 20min by using high-pressure steam at 120 ℃ and 110kpa, cooling to 50-60 ℃, and preserving at constant temperature for later use;
2.3 testing (diffusion method)
Blank control group: purified water (cooled to room temperature after autoclaving)
Taking 5 groups (group 1, group 2, group 3, group 4 and group 5) of culture dishes filled with solid culture media, uniformly coating liquid culture media on the culture media of each culture dish, respectively and correspondingly inoculating the 5 bacteria (group 1 (inoculated with staphylococcus aureus), group 2 (inoculated with candida albicans), group 3 (inoculated with streptococcus mutans), group 4 (inoculated with lactobacillus) and group 5 (inoculated with porphyromonas gingivalis)) on each culture dish, and then placing the culture dishes in a constant-temperature incubator at 37 ℃ for 24 hours to obtain culture dishes;
weighing 50mg of the mouthwash prepared in the examples 1 to 4 and 50mg of the purified water of the blank control group, respectively dripping the 50mg of the purified water of the blank control group on 15 small circular filter paper sheets by using a 10 mu L capillary dropper in an equal amount, and uniformly and symmetrically attaching 3 small circular filter paper sheets (containing the same type of mouthwash or the blank control group) to each culture dish, wherein 3 small circular filter paper sheets of the same type of mouthwash or the blank control group are respectively and uniformly attached to 5 tissue culture dishes (containing one culture dish of each group) in each culture dish by taking 3 small circular filter paper sheets as a small group, and 3 small circular filter paper sheets in each culture dish are uniformly and symmetrically attached to a central area of a culture medium in the corresponding culture dish;
after the culture dishes with the small disks attached thereto were placed in a constant temperature incubator at 37 ℃ for 24 hours, the diameters of three quasi-circular antibacterial areas in each dish were measured and averaged, as specifically shown in table 1:
TABLE 1 average diameter of antimicrobial region
Figure BDA0001952092750000081
And (3) performing an antibacterial test by adopting a diffusion method, if the corresponding sample has antibacterial property, displaying an antibacterial area on the culture medium, evaluating the antibacterial property of the sample according to the diameter of the antibacterial area, wherein the larger the diameter is, the stronger the antibacterial property is. Wherein, the staphylococcus aureus, the candida albicans, the streptococcus mutans, the lactobacillus and the porphyromonas gingivalis are common oral bacteria, the staphylococcus aureus is a gram-negative coccus, is usually piled into a grape string shape and is easy to cause oral inflammation, the candida albicans is a fungus, is usually present in the oral cavity and the upper respiratory tract of a normal person, is easy to invade cells to cause diseases when the immune function of a human body is reduced, the streptococcus mutans is one of the main components of dental plaque and is also the main pathogenic bacteria of caries, the caries is a bacterial infectious disease occurring in hard tissues of teeth, the incidence rate is highest in oral diseases, the lactobacillus refers to the bacteria which can ferment saccharides to generate lactic acid, the lactobacillus ferments the saccharides to generate a large amount of lactic acid and is easy to cause caries, the porphyromonas gingivalis is a gram-negative anaerobic bacillus which is not used for decomposing the saccharides and is one of periodontal pathogenic bacteria, once out of control, Porphyromonas gingivalis can cause the gingiva to fall off the teeth.
As can be seen from Table 1, the blank control group (purified water) does not show the antibacterial region, while the mouth rinses prepared in examples 1-3 all generate obvious antibacterial regions for 5 common bacteria such as Staphylococcus aureus, Candida albicans, Streptococcus mutans, Lactobacillus, Porphyromonas gingivalis, and example 4 has obviously better inhibitory effect on Staphylococcus aureus and Candida albicans than examples 1-3, the main reason is that in the embodiment 4, dry leaf steam distillation is respectively carried out on the fresh agastache rugosus leaves to obtain agastache rugosus essential oil, the fresh leaves are pulped and then are subjected to freezing extraction to obtain a first extract, and the pseudo-ginseng and the lonicera confusa are matched to be boiled in water and subjected to alcohol precipitation to obtain the traditional Chinese medicine composition extract, so that the extraction amount of the agastache rugosus ketone, the cinnamaldehyde and the like in the agastache rugosus can be effectively increased, and the bacteriostatic effect of the mouthwash on staphylococcus aureus and candida albicans is improved.
3. Clinical observations
3.1 adopting the opinion score method
Selecting 40 patients with gingival pain caused by gingivitis as experimental objects, randomly dividing the experimental objects into 2 groups (including an experimental group 1 and an experimental group 2, wherein each group comprises 20 persons), and using the mouthwash by each person after three meals and before sleep, wherein the mouthwash prepared in example 1 is used in the experimental group 1, the mouthwash prepared in example 5 is used in the experimental group 2, and the use method of the mouthwash is as follows: holding 15-20mL of mouthwash in the mouth, pumping the cheeks and lips for 40s to make the mouthwash fully contact with teeth and gums in the oral cavity, and repeatedly rinsing each part of the oral cavity without eating or drinking within 30 min.
2 days as a course of treatment, recording and counting the relief of gingival pain symptoms, as shown in table 2:
TABLE 2 relief of gingival pain symptoms caused by gingivitis
Figure BDA0001952092750000091
As can be seen from table 2, the mouth wash prepared in example 1 and the mouth wash prepared in example 5 both released the pain sensation in the mouth caused by gingivitis, wherein the release effect of example 5 was superior to that of example 1.
3.3 adopting the opinion score method
40 patients with gingival pain caused by periodontitis were selected as experimental subjects, randomly divided into 2 groups (including experimental group 1 and experimental group 2, each group consisting of 20 persons), and used with the mouth wash after three meals and before sleep, wherein the experimental group 1 used the normal saline on the basis of the oral anti-inflammatory drug, and the experimental group 2 used the mouth wash prepared in example 5 on the basis of the oral anti-inflammatory drug, and the usage methods of the normal saline and the mouth wash were as follows: holding 15-20mL of mouthwash or normal saline in the mouth, pumping the cheek and the lip for 40s to make the mouthwash or normal saline in the mouth fully contact with the teeth and gum, and repeatedly rinsing each part of the mouth without eating or drinking within 30 min.
1 day is a treatment course, and the relief condition of the gingival pain symptom is recorded and counted, which is specifically shown in table 2:
TABLE 2 relief of gingival pain symptoms caused by periodontitis
Days of use Experimental group 1 Experimental group 2
1 12 people relieve oral cavity pain 4 obviously improving the pain feeling of the oral cavity
2 4 obviously improving the pain feeling of the oral cavity 7 obviously improves the pain feeling of the oral cavity
3 6 obviously improves the pain feeling of the oral cavity The 12 people obviously improve the pain feeling of the oral cavity
As can be seen from Table 3: the oral anti-inflammatory drug for patients with periodontitis and the mouth wash prepared in example 5 has better effect of relieving oral cavity pain than the oral anti-inflammatory drug and normal saline.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.

Claims (4)

1. The compound traditional Chinese medicine mouthwash is characterized by comprising the following raw materials in parts by weight:
12-15% of traditional Chinese medicine composition extract, 0.01-1% of sweetening agent, 0.02-1% of sour agent, 2-10% of humectant, 0.01-0.4% of preservative, 0.5-5% of menthol and the balance of water, wherein the raw material medicines of the traditional Chinese medicine extract comprise: 20-23 parts of agastache rugosus, 12-15 parts of lonicera confusa and 2-3 parts of pseudo-ginseng;
the preparation method of the compound traditional Chinese medicine mouthwash comprises the following steps:
s1, dividing the fresh agastache rugosus leaves into three parts;
one part of fresh agastache rugosus leaves are dried in a 65 ℃ oven to constant weight after being dried in the sun and nightly for 3-4 days continuously, ground into powder and sieved by a 200-mesh sieve at 100 ℃, so as to obtain agastache rugosus powder, water with the amount of 8 times of the total mass of the powder is added into the powder, and the powder is soaked for 5 hours and then subjected to steam distillation extraction for 4 hours, so as to obtain agastache rugosus essential oil;
adding 0.05 times of lemon juice and 1 time of water into the other part of fresh agastache rugosus leaf, pulping to obtain a pulp, cooling the pulp to-20 ℃, keeping the temperature for 3 hours, taking out the pulp, thawing at room temperature to obtain a frozen pulp, adding 2 times of water into the frozen pulp, filtering to obtain a first filtrate and a first filter residue, adding 4 times of water into the first filtrate, stirring for 10 minutes, filtering to obtain a second filtrate, combining the first filtrate and the second filtrate, and concentrating to obtain a first extract;
sun drying the last fresh folium Agastaches until the water content is less than 12% to obtain dry folium Agastaches, and mixing dry folium Agastaches, flos Lonicerae and Notoginseng radix to obtain Chinese medicinal mixture;
adding water 15 times the total mass of the Chinese medicinal mixture, boiling and extracting for 2 times, the first time for 2 hours, the second time for 1.5 hours, combining the filtrate obtained by 2 times of extraction, concentrating under reduced pressure to obtain a concentrated solution, adding ethanol into the concentrated solution to make the alcohol content reach 60%, stirring, uniformly mixing, standing for 24 hours, filtering to remove precipitate to obtain an alcohol precipitation filtrate, and concentrating the alcohol precipitation filtrate to obtain a Chinese medicinal composition extract;
s2, mixing the Chinese medicinal extract, herba Agastaches essential oil, the first extract, sweetener, sour agent, humectant, antiseptic, menthol and water, and packaging.
2. The compound traditional Chinese medicine mouth wash as claimed in claim 1, wherein the sweetener is one or more of sucralose, fructose and stevioside, the sour agent is one of malic acid, citric acid and tartaric acid, the humectant is one of glycerin and sorbitol, and the preservative is one or more of methyl paraben, ethyl paraben and sodium benzoate.
3. The compound traditional Chinese medicine mouth wash as claimed in claim 2, wherein the specific gravity of the concentrated solution in step S1 at 80 ℃ is 1.02-1.10, and the specific gravity of the traditional Chinese medicine combined extract at 80 ℃ is 1.06-1.12.
4. The compound traditional Chinese medicine mouth wash as claimed in claim 3, wherein the bulk drugs of the traditional Chinese medicine extract further comprise: 7-8 parts of pepper and 2-5 parts of eupatorium fortunei, and the step S1 further comprises the following steps:
weighing 7-8 parts of pepper, grinding into powder, adding water with the amount being 10 times of the total mass of the pepper, boiling and extracting for 2 times, 2 hours for the first time and 1 hour for the second time, combining filtrate obtained by 2 times of extraction, and concentrating to obtain a second extract;
weighing 2-5 parts of eupatorium fortunei, grinding into powder, adding water with the amount being 10 times of the total mass of the eupatorium fortunei, boiling and extracting for 2 times, the first time for 3 hours and the second time for 2 hours, combining filter liquor extracted for 2 times, concentrating to obtain a third extract, adding water to dilute the third extract, then carrying out alcohol precipitation, stirring and uniformly mixing, standing for 2 hours, filtering to obtain a first alcohol precipitate, adding water to dissolve the first alcohol precipitate, then carrying out alcohol precipitation, stirring and uniformly mixing, standing for 2 hours, and filtering to obtain a second alcohol precipitate;
step S2 is to mix the Chinese medicinal extract, herba Agastaches essential oil, first extract, second alcohol precipitate, sweetener, sour agent, humectant, antiseptic, menthol and water thoroughly, and subpackage.
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