CN111529475A - Compound rehabilitation new liquid mouth wash and preparation method thereof - Google Patents
Compound rehabilitation new liquid mouth wash and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a compound rehabilitation new liquid mouthwash and a preparation method thereof. The compound new liquid mouthwash is prepared from a mixed fluid extract filtrate and a rehabilitation new liquid according to the volume ratio of (2-10): 50, and the mixed fluid extract is prepared by mixing a honeysuckle fluid extract, a chrysanthemum fluid extract, a dandelion fluid extract and a mint fluid extract. The preparation method comprises mixing the mixed fluid extract filtrate and the rehabilitation new liquid according to formula ratio, and stirring well to obtain the final product. The invention extracts and mixes fluid extracts from four medicaments of honeysuckle, chrysanthemum, dandelion and mint respectively, prepares a compound rehabilitation new traditional Chinese medicine mouthwash formula with a rehabilitation new liquid in different proportioning modes, preliminarily determines the formula by comparing the properties of the formula in aspects of properties, colors, mouthfeel and the like, checks whether the formula damages enamel and has antibacterial effect through safety experiments and antibacterial experiments, and provides a theoretical basis for further developing safe and effective natural medicament oral compound preparation mouthwash.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to compound rehabilitation new liquid mouthwash and a preparation method thereof.
Background
In China, natural medicines have long application history, small toxic and side effects, convenient material taking, economy and practicability, and some medicines also have the effects of sterilization and inflammation diminishing, so the natural medicines are widely used for basic research and clinical practice. The Chinese medicinal preparation has wide application in oral diseases, and a large number of researches show that the Chinese medicinal preparation has good curative effect on treating diseases such as periodontal diseases, oral ulcer and the like. Along with the concern of people on the safety of the mouthwash, the advantages of the traditional Chinese medicine mouthwash are gradually shown.
Disclosure of Invention
The first purpose of the invention is to provide a compound rehabilitation new liquid mouth wash; the second purpose is to provide a preparation method of the compound rehabilitation new liquid mouth wash.
The first purpose of the compound new liquid mouthwash is achieved by preparing mixed fluid extract filtrate and new rehabilitation liquid according to the volume ratio of (2-10): 50, wherein the mixed fluid extract is prepared by mixing honeysuckle fluid extract, chrysanthemum fluid extract, dandelion fluid extract and mint fluid extract.
The second purpose of the invention is realized by that the preparation method of the compound rehabilitation new liquid mouth wash is obtained by mixing and stirring the mixed fluid extract filtrate and the rehabilitation new liquid uniformly according to the formula proportion.
On the basis of the 'new recovery liquid', four traditional Chinese medicines of honeysuckle, chrysanthemum, mint and dandelion are compatible, and by utilizing respective drug effects and synergistic effects of the five medicines, the compound new recovery traditional Chinese medicine mouthwash which has the auxiliary treatment effect on oral mucosa diseases, such as bacteriostasis, anti-inflammation, breath freshening, wound healing promotion and the like, is safe and nontoxic is expected to be prepared. Lays a foundation for the traditional Chinese medicine in the field of mouthwash industry, thereby expanding the application field of the traditional Chinese medicine.
The new healing liquid is a common medicine for surgery, is suitable for treating wounds, pressure sores, burns, incised sores, fistulas and scalds, has the effects of nourishing yin, promoting granulation and promoting blood circulation, can improve the immune function of patients, and has an activation effect on nonspecific immune function cells. The new rehabilitation liquid is a pure natural medicine extracted from dried periplaneta americana by alcohol, and contains bioactive components such as polyol and peptide active substances including 18 amino acids. Compared with the traditional western medicine, the traditional Chinese medicine composition has the advantages of high safety, small side effect, convenience in use, difficulty in generating drug resistance and the like. The traditional Chinese medicine composition is also applied to treatment of oral ulcer at present, is a main treatment method and treatment means, and has typical application value in stomatology. Korean red Juan-Zi and Wuhao, etc[8]The experimental results of the comparison and analysis of the curative effects of the novel rehabilitation liquid and the benefiting buccal tablet on treating the dental ulcer show that the novel rehabilitation liquid has better curative effect on treating the dental ulcer, and provides a powerful basis for the novel rehabilitation liquid to treat the dental ulcer.
The flos Lonicerae is Lonicera Japonica flos (Lonicera Japonica flos, LoLonicera japonicaThunb.) or a flower with an initial bloom. Honeysuckle is known as a good medicine for clearing heat and removing toxicity from the old, and has obvious effects on various heat diseases, such as body heat, eruption, macula, heat-toxin sores and carbuncles, sore throat and the like. Modern researches prove that the honeysuckle has a good treatment effect on the dental ulcer, and the honeysuckle contains pharmacological active ingredients such as chlorogenic acid and the like, so that the honeysuckle has a good antibacterial effect. The research of ancient red plum and royal red star shows that the honeysuckle has good bacteriostatic action on staphylococcus aureus and escherichia coli.
The flos Chrysanthemi is Compositae plant flos Chrysanthemi (Chrysanthemum morifolium Ramat.)Chrysanthemum morifoliumRamat.) belonging to the family of wild chrysanthemum together with wild chrysanthemum. The chrysanthemum is sweet, bitter and slightly cold in taste, and has the effects of dispelling wind, clearing heat, calming liver, improving eyesight, clearing heat and detoxifying. It can be used for treating headache, vertigo, conjunctival congestion, dysphoria with smothery sensation in chest, furuncle, and toxic swelling. Chrysanthemum flowerThe flower contains volatile oil, flavonoids, polysaccharides, diterpenes, phenolic acid, etc., wherein the flavonoids and volatile oil are abundant. The wild chrysanthemum extract has the effects of resisting pathogenic microorganisms, resisting inflammation, improving immunity, protecting cardiovascular system, resisting tumor and the like, and researches show that the wild chrysanthemum extract stock solution has strong bacteriostatic activity on pathogenic bacteria in the oral cavity such as staphylococcus aureus, escherichia coli, salmonella and the like.
Herba Taraxaci is Compositae herba Taraxaci (Taraxacum mongolicum hand. -Mazz.)Taraxacum mongolicumHand. -Mazz.), herb of Latifolia Delavayi, herb of Latica veronica, etc. Herba Taraxaci has effects of clearing heat and detoxicating, subsiding swelling and resolving hard mass, inducing diuresis and freeing strangury, and can be used for treating furuncle pyogenic infections, acute mastitis, scrofula, conjunctival congestion, pharyngalgia, pulmonary abscess, intestinal abscess, damp-heat jaundice, and stranguria with astringency and pain. It is widely distributed and can grow in spring, summer and autumn mainly in the areas of north China, east China, northeast China and the like. Researches on plum army, wang Yongli and the like have proved that dandelion can effectively shorten the healing time of canker sore. Chenna, Wandongxue and the like draw the conclusion that the chlorogenic acid extracting solution in the dandelion has stronger antibacterial activity and can better inhibit the growth activity of staphylococcus aureus and escherichia coli.
The herba Menthae is herba Menthae (Mentha haplocalyx, Mentha hapMentha haplocalyxBriq.)). The whole plant is green and fragrant, and is one of the traditional Chinese medicines commonly used in China. It is a pungent and cool sweating antipyretic, and can be used for treating influenza, headache, conjunctival congestion, fever, and swelling and pain of throat and gum. It can be used for treating neuralgia, skin pruritus, erythra, eczema, etc. Research shows that the mint water extract has obvious bacteriostatic activity on escherichia coli, staphylococcus aureus, bacillus subtilis and salmonella, wherein the mint water extract has the best inhibitory effect on staphylococcus aureus, and the mint has a good bacteriostatic effect.
The theory of traditional Chinese medicine considers that: the oral ulcer is caused by internal injury due to seven emotions, asthenia, and external infection of six excesses, which causes stagnation of liver qi, stagnated heat transforming into fire, intense heart fire, stomach fire attacking upwards, disharmony between heart and kidney, and flaring-up of deficient fire fumigating the mouth. The immunity of the organism is reduced along with the activity, alternation and overlapping of one or more factors, and the immune function is disordered, thereby causing the frequent onset of the oral ulcer. The novel rehabilitation liquid, the honeysuckle, the chrysanthemum, the dandelion and the mint have strong biological activity and are proved to have the effects of inhibiting bacteria and effectively preventing and treating dental ulcer, but the 5 medicines are compounded and applied to the adjuvant therapy of the dental ulcer diseases, and no report is found yet.
The invention extracts fluid extracts from honeysuckle, chrysanthemum, dandelion and mint respectively, obtains mixed fluid extracts according to the proportion of 1:1:1:1, prepares a compound rehabilitation new traditional Chinese medicine mouthwash formula with a rehabilitation new liquid in different proportioning modes, preliminarily determines the formula by comparing the properties of the formula in aspects of properties, colors, mouthfeel and the like, checks whether the formula damages enamel and has antibacterial effect or not through safety experiments and antibacterial experiments, and provides theoretical basis for further developing safe and effective natural medicine compound oral mouthwash.
The invention extracts the medicinal materials by refluxing 75% ethanol and 80% ethanol, measures the specific gravity value of the fluid extract after the concentration of the medicinal material extracting solution as an investigation index, and screens out the optimal extraction process of each medicinal material if the specific gravity value is higher, which indicates that the extraction rate of the medicinal material is higher.
1. The process design for extracting honeysuckle by 75% ethanol comprises the following steps:
extracting for the first time: adding 15 times of solvent, refluxing for 1 hr, and filtering to obtain filtrate
And (3) performing secondary extraction on 100g of medicinal materials: adding 12 times of solvent, refluxing for 1 hr, and filtering to obtain filtrate
And (3) extracting for the third time: adding 10 times of solvent, refluxing for 1 hr, and filtering to obtain filtrate
And (3) fourth extraction: adding 10 times of solvent, refluxing for 1 hr, and filtering to obtain filtrate
Mixing filtrates, concentrating under reduced pressure to obtain 50ml fluid extract, and measuring specific gravity with hydrometer
Extracting for the first time: adding 15 times of solvent, refluxing for 1 hr, and filtering to obtain filtrate
And (3) performing secondary extraction on 100g of medicinal materials: adding 12 times of solvent, refluxing for 1 hr, and filtering to obtain filtrate
And (3) extracting for the third time: adding 10 times of solvent, refluxing for 1 hr, and filtering to obtain filtrate
Mixing filtrates, concentrating under reduced pressure to obtain 50ml fluid extract, and measuring specific gravity with hydrometer
2. The process design for extracting honeysuckle by 80% ethanol comprises the following steps:
extracting for the first time: refluxing with 15 times of solvent for 40min, and filtering to obtain filtrate
And (3) performing secondary extraction on 100g of medicinal materials: adding 12 times of solvent, refluxing for 40min, and filtering to obtain filtrate
And (3) extracting for the third time: adding 10 times of solvent, refluxing for 40min, and filtering to obtain filtrate
The filtrates were combined, concentrated under reduced pressure to 50ml of fluid extract, and the specific gravity was measured with a densitometer.
The extraction process of the chrysanthemum, the dandelion and the mint is the same as that of the honeysuckle.
And the specific gravity data of the fluid extract measured by the three-time extraction process of each medicinal material
The specific gravity value of the fluid extract measured by three-time extraction process of each medicinal material
4. Mouthwash formulation and property comparison
Mixing flos Lonicerae fluid extract, flos Chrysanthemi fluid extract, herba Taraxaci fluid extract and herba Menthae fluid extract at a ratio of 1:1:1:1 to obtain mixed fluid extract, dissolving the mixed fluid extract in 75% medical ethanol, adding activated carbon for decolorizing, filtering while hot, and mixing the filtrate with the new rehabilitation liquid to obtain the final product. The prepared formula is used for preliminarily screening out a formula suitable for being used as mouthwash according to the characteristics, the color and the taste of three types of mouthwash of the plum schliederin cool and refreshing mouthwash, the Gaolujie Beidongqing tea health mouthwash and the Shuke professional refreshing mouthwash (see embodiment 1 specifically).
Drawings
FIG. 1 is a schematic diagram of a safety review test for formulation A2 of the present invention;
FIG. 2 is a schematic diagram of a safety review test for formulation A3 of the present invention;
FIG. 3 is a schematic diagram of a safety review test for formulation A4 of the present invention;
FIG. 4 is a schematic of a safety review test for formulation A5 of the present invention;
FIG. 5 is a schematic of a safety review test for formulation A6 of the present invention;
FIG. 6 is a schematic of a safety review test for formulation A7 of the present invention;
FIG. 7 is a schematic of a safety review test for formulation A8 of the present invention;
FIG. 8 is a schematic of a safety review test for formulation A9 of the present invention;
FIG. 9 is a schematic of a safety review test for formulation A10 of the present invention;
FIG. 10 is a schematic diagram of 1ml of E.coli added in the formulation A10 according to the invention;
FIG. 11 is a schematic representation of 1ml of Staphylococcus aureus added in a formulation A10 according to the invention;
FIG. 12 is a schematic diagram of 2ml of E.coli added in the formulation A10 according to the present invention;
FIG. 13 is a schematic representation of 2ml of Staphylococcus aureus added in a formulation A10 according to the invention;
FIG. 14 is a schematic diagram of 3ml of E.coli added in formulation A10 according to the invention;
FIG. 15 is a schematic representation of 3ml of Staphylococcus aureus added in a formulation A10 according to the invention;
FIG. 16 is a schematic diagram of E.coli in a dose of 4ml according to formulation A10 of the present invention;
FIG. 17 is a schematic representation of 4ml of Staphylococcus aureus dosed in formulation A10 according to the invention;
FIG. 18 is a schematic of 5ml of E.coli added in formulation A10 according to the invention;
FIG. 19 is a schematic representation of 5ml of Staphylococcus aureus added in formulation A10 according to the invention;
FIG. 20 is a schematic diagram of 1ml of E.coli added in a formulation A2 according to the invention;
FIG. 21 is a schematic representation of 1ml of Staphylococcus aureus added in a formulation A2 according to the invention;
FIG. 22 is a schematic diagram of 2ml of E.coli dosed with formulation A2 according to the invention;
FIG. 23 is a schematic representation of 2ml of Staphylococcus aureus added in a formulation A2 according to the invention;
FIG. 24 is a schematic diagram of 3ml of E.coli added in formulation A2 according to the invention;
FIG. 25 is a schematic representation of 3ml of Staphylococcus aureus added in formulation A2 according to the invention;
FIG. 26 is a schematic diagram of E.coli in a dose of 4ml according to formulation A2 of the present invention;
FIG. 27 is a schematic representation of 4ml of Staphylococcus aureus dosed in formulation A2 according to the invention;
FIG. 28 is a schematic of 5ml of E.coli added in formulation A2 according to the invention;
FIG. 29 is a schematic representation of 5ml of Staphylococcus aureus added in a formulation A2 according to the invention;
FIG. 30 is a schematic diagram of Escherichia coli added with 5ml of convalescent liquid;
FIG. 31 is a schematic diagram of Staphylococcus aureus added with 5ml volume of the healing tonic.
Detailed Description
The present invention is further illustrated by the following examples and the accompanying drawings, but the present invention is not limited thereto in any way, and any modifications or alterations based on the teaching of the present invention are within the scope of the present invention.
The compound new liquid mouthwash is prepared from a mixed fluid extract filtrate and a rehabilitation new liquid according to the volume ratio of (2-10): 50, wherein the mixed fluid extract is prepared by mixing a honeysuckle fluid extract, a chrysanthemum fluid extract, a dandelion fluid extract and a mint fluid extract.
The mass ratio of the honeysuckle fluid extract to the chrysanthemum fluid extract to the dandelion fluid extract to the mint fluid extract is (0.5-1.5): 0.5-1.5).
The mass ratio of the honeysuckle fluid extract to the chrysanthemum fluid extract to the dandelion fluid extract to the mint fluid extract is 1:1:1: 1.
The honeysuckle fluid extract is obtained by carrying out reflux extraction on 75% ethanol or 80% ethanol, and the specific operation is as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of honeysuckle medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target honeysuckle fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the honeysuckle medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with the volume 12 times that of the honeysuckle medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain a filtrate g and a filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target honeysuckle fluid extract;
the second method comprises the following steps:
taking 100g of honeysuckle medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target honeysuckle fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of flos Lonicerae, reflux extracting for 1h to obtain filtrate a and residue b;
2) adding 75% ethanol with the volume 12 times that of the honeysuckle medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target honeysuckle fluid extract;
B. extracting with 80% ethanol:
taking 100g of honeysuckle medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target honeysuckle fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of flos Lonicerae, reflux extracting for 1h to obtain filtrate a and residue b;
2) adding 80% ethanol with the volume 12 times that of the honeysuckle medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target honeysuckle fluid extract.
The chrysanthemum fluid extract is obtained by carrying out reflux extraction on 75% ethanol or 80% ethanol, and the specific operation is as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of chrysanthemum medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target chrysanthemum fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the chrysanthemum medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the chrysanthemum medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain filtrate g and filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target chrysanthemum fluid extract;
the second method comprises the following steps:
taking 100g of chrysanthemum medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target chrysanthemum fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of the chrysanthemum medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the chrysanthemum medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target chrysanthemum fluid extract;
B. extracting with 80% ethanol:
taking 100g of chrysanthemum medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target chrysanthemum fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of flos Chrysanthemi, reflux extracting for 1h to obtain filtrate a and residue b;
2) adding 80% ethanol with volume 12 times of that of the chrysanthemum medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target chrysanthemum fluid extract.
The dandelion fluid extract is obtained by carrying out reflux extraction on 75% ethanol or 80% ethanol, and the specific operation is as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of dandelion medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target dandelion fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the dandelion herb, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the dandelion herb into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain filtrate g and filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target dandelion fluid extract;
the second method comprises the following steps:
taking 100g of dandelion medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target dandelion fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of the dandelion herb, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the dandelion herb into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target dandelion fluid extract;
B. extracting with 80% ethanol:
taking 100g of dandelion medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target dandelion fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of the dandelion herb, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 80% ethanol with volume 12 times of that of the dandelion herb into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target dandelion fluid extract.
The mint fluid extract is obtained by carrying out reflux extraction on 75% ethanol or 80% ethanol, and the specific operation is as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of mint medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target mint fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the mint medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the mint medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the mint medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the mint medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain a filtrate g and a filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target mint fluid extract;
the second method comprises the following steps:
extracting 100g of mint medicinal materials for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target mint fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of the herba Menthae, reflux-extracting for 1h to obtain filtrate a and residue b;
2) adding 75% ethanol with volume 12 times of that of the mint medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the mint medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target mint fluid extract;
B. extracting with 80% ethanol:
extracting 100g of mint medicinal materials for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target mint fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of the herba Menthae, reflux-extracting for 1h to obtain filtrate a and residue b;
2) adding 80% ethanol with volume 12 times of that of the mint medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the mint medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target mint fluid extract.
The mixed fluid extract filtrate is obtained by dissolving the mixed fluid extract in 75% ethanol, adding activated carbon for decoloring, and filtering while hot.
The preparation method of the compound rehabilitation new liquid mouthwash is obtained by mixing and stirring the mixed fluid extract filtrate and the rehabilitation new liquid uniformly according to the formula ratio.
The invention is further illustrated by the following specific examples:
example 1
Adding 80g of the mixed fluid extract into 500ml of 75% medical ethanol, heating for dissolving, adding 20g of activated carbon for decoloring, filtering while hot, and matching and comparing the obtained filtrate with the rehabilitation new liquid, wherein the specific steps are as follows:
mixing ratio of fluid extract filtrate and rehabilitation new liquid
Comparison of properties of mouthwash formulas with different ratio numbers
Example 2
And (3) investigating the safety of the formula:
the prepared formulation, numbered A2-A10, was autoclaved for 30 min (temperature 121 ℃).
Some components contained in the test formulation may cause damage such as dissolution and abrasion to the enamel surface or the filler surface of the tooth, resulting in a decrease in the microhardness or a change in the surface topography of the enamel or filler surface.
19 whole teeth were selected from human teeth taken from the stomatology department, labeled and recorded by photography. The teeth numbered 1-19 were placed in the A2-A10 formulation and recorded (see appendix 2):
the teeth numbered 1, 2 were placed in the a2 formulation; the teeth numbered 3 and 4 were placed in the a3 formulation;
the teeth numbered 5 and 6 were placed in the a4 formulation; the teeth numbered 7 and 8 were placed in the a5 formulation;
the teeth numbered 9, 10 were placed in the a6 formulation; the teeth numbered 11, 12 were placed in the a7 formulation;
the tooth number 13 was placed in the A8 formulation (the tooth number 14 was larger than the mouth and was not placed in, so no record was made);
the teeth numbered 15, 16 were placed in the a9 formulation; the teeth numbered 17, 18, 19 were placed in the a10 formulation.
After one week of placement, each formulation was observed for tooth condition and compared to tooth condition before placement.
By observation, the soaked teeth had deposits that adhered to and were consistent with the original color after rinsing, and thus, the prepared mouthwash did not cause a reduction in the surface microhardness or a change in the surface topography of the enamel or filling, and all formulations did not dissolve or erode the enamel surface of the teeth.
Example 3
And (3) effectiveness investigation:
and (4) carrying out an antibacterial test by using the prepared mouthwash, and inspecting whether the sample has an antibacterial effect.
Qualitative research of bacteriostasis
The oral ulcer is related to the change of the quantity of gram-negative cocci, streptococcus and veillonella in the oral cavity, and the reports show that the rehabilitation new liquid, honeysuckle, chrysanthemum, dandelion and mint have good antibacterial effect. The experiment aims to adopt staphylococcus aureus and escherichia coli as targets, preliminarily researches the inhibition effect of the compound rehabilitation new traditional Chinese medicine mouthwash formula on the two bacteria, and provides a foundation for the development of the next experiment.
Activated culture of strain and preparation of bacterial liquid
The broth is prepared by mixing nutrient broth culture medium dry powder and distilled water at a ratio of 11:500, and autoclaving at 121 deg.C for 0.5 h. Pouring into a culture dish, cooling, and placing into a refrigerator for later use. Respectively inoculating Escherichia coli and Staphylococcus aureus to nutrient broth culture medium, culturing at 37 deg.C for 24 hr, and preparing into 1.5 × 108 CFU/mL bacterial suspension by turbidimetry with sterile physiological saline.
Bacteriostatic qualitative experiment-medicated plate method
And (5) preparing a drug-containing flat plate, and carrying out bacteriostasis experiment detection on the rehabilitation new liquid, the formulas A2 and A10.
Mixing the nutrient agar culture medium dry powder with distilled water, mixing the nutrient agar culture medium dry powder with the distilled water at a ratio of 19: 500, sterilizing at 121 ℃ for 0.5h, taking out, respectively adding 1ml, 2ml, 3ml, 4ml, 5ml and 5 doses of formula samples and 5ml of rehabilitation new liquid into a culture dish, pouring a culture medium into the culture dish with the formula samples and the rehabilitation new liquid, uniformly mixing the samples and the culture medium, naturally cooling, and putting into a refrigerator for later use.
The surface of a culture medium containing the medicine is dipped with an aseptic cotton swab to obtain escherichia coli liquid (staphylococcus aureus liquid), the escherichia coli liquid is uniformly coated on the culture medium once per 60-degree rotation, the escherichia coli liquid is coated for three times in total, and finally, the edge of the culture medium is wound for one circle. And finally, putting the culture medium into an incubator to be cultured for 24 hours, and observing the growth condition of the bacterial colony on the surface of the culture medium.
Experimental results show that the prepared compound rehabilitation new traditional Chinese medicine mouthwash formula has an antibacterial effect on staphylococcus aureus and escherichia coli.
Claims (9)
1. The compound new rehabilitation liquid mouthwash is characterized by being prepared from a mixed fluid extract filtrate and new rehabilitation liquid according to a volume ratio of (2-10): 50, wherein the mixed fluid extract is prepared by mixing a honeysuckle fluid extract, a chrysanthemum fluid extract, a dandelion fluid extract and a mint fluid extract.
2. The compound rehabilitation new liquid mouthwash according to claim 1, wherein the mass ratio of the honeysuckle fluid extract, the chrysanthemum fluid extract, the dandelion fluid extract and the mint fluid extract is (0.5-1.5): (0.5-1.5).
3. The compound rehabilitation new liquid mouthwash according to claim 1 or 2, wherein the mass ratio of the honeysuckle fluid extract, the chrysanthemum fluid extract, the dandelion fluid extract and the mint fluid extract is 1:1:1: 1.
4. The compound rehabilitation new liquid mouthwash according to claim 1 or 2, wherein the honeysuckle fluid extract is obtained by reflux extraction with 75% ethanol or 80% ethanol, and the specific operations are as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of honeysuckle medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target honeysuckle fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the honeysuckle medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with the volume 12 times that of the honeysuckle medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain a filtrate g and a filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target honeysuckle fluid extract;
the second method comprises the following steps:
taking 100g of honeysuckle medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target honeysuckle fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of flos Lonicerae, reflux extracting for 1h to obtain filtrate a and residue b;
2) adding 75% ethanol with the volume 12 times that of the honeysuckle medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target honeysuckle fluid extract;
B. extracting with 80% ethanol:
taking 100g of honeysuckle medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target honeysuckle fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of flos Lonicerae, reflux extracting for 1h to obtain filtrate a and residue b;
2) adding 80% ethanol with the volume 12 times that of the honeysuckle medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the honeysuckle medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target honeysuckle fluid extract.
5. The compound new rehabilitation liquid mouthwash according to claim 1, wherein the chrysanthemum fluid extract is obtained by reflux extraction with 75% ethanol or 80% ethanol, and the specific operations are as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of chrysanthemum medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target chrysanthemum fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the chrysanthemum medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the chrysanthemum medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain filtrate g and filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target chrysanthemum fluid extract;
the second method comprises the following steps:
taking 100g of chrysanthemum medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target chrysanthemum fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of the chrysanthemum medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the chrysanthemum medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target chrysanthemum fluid extract;
B. extracting with 80% ethanol:
taking 100g of chrysanthemum medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target chrysanthemum fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of flos Chrysanthemi, reflux extracting for 1h to obtain filtrate a and residue b;
2) adding 80% ethanol with volume 12 times of that of the chrysanthemum medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the chrysanthemum medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target chrysanthemum fluid extract.
6. The compound rehabilitation new liquid mouthwash according to claim 1, wherein the dandelion fluid extract is obtained by reflux extraction with 75% ethanol or 80% ethanol, and the specific operations are as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of dandelion medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target dandelion fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the dandelion herb, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the dandelion herb into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain filtrate g and filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target dandelion fluid extract;
the second method comprises the following steps:
taking 100g of dandelion medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target dandelion fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of the dandelion herb, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the dandelion herb into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target dandelion fluid extract;
B. extracting with 80% ethanol:
taking 100g of dandelion medicinal material, extracting for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target dandelion fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of the dandelion herb, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 80% ethanol with volume 12 times of that of the dandelion herb into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the dandelion medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target dandelion fluid extract.
7. The compound rehabilitation new liquid mouthwash according to claim 1, wherein the mint fluid extract is obtained by reflux extraction with 75% ethanol or 80% ethanol, and the specific operations are as follows:
A. extracting with 75% ethanol:
the method comprises the following steps:
taking 100g of mint medicinal material, extracting for four times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target mint fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times the volume of the mint medicinal material, and performing reflux extraction for 1h to obtain filtrate a and filter residue b;
2) adding 75% ethanol with volume 12 times of that of the mint medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the mint medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
4) adding 75% ethanol with the volume 10 times that of the mint medicinal material into the filter residue f, and performing reflux extraction for 1h to obtain a filtrate g and a filter residue h;
5) mixing the filtrate a, the filtrate c, the filtrate e and the filtrate g, and concentrating under reduced pressure to obtain a target mint fluid extract;
the second method comprises the following steps:
extracting 100g of mint medicinal materials for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target mint fluid extract, wherein the extraction steps are as follows:
1) adding 75% ethanol 15 times of the herba Menthae, reflux-extracting for 1h to obtain filtrate a and residue b;
2) adding 75% ethanol with volume 12 times of that of the mint medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 75% ethanol with the volume 10 times that of the mint medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
mixing the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain a target mint fluid extract;
B. extracting with 80% ethanol:
extracting 100g of mint medicinal materials for three times, combining filtrates, and concentrating under reduced pressure to 50ml to obtain a target mint fluid extract, wherein the extraction steps are as follows:
1) adding 80% ethanol 15 times of the herba Menthae, reflux-extracting for 1h to obtain filtrate a and residue b;
2) adding 80% ethanol with volume 12 times of that of the mint medicinal material into the filter residue b, and performing reflux extraction for 1h to obtain filtrate c and filter residue d;
3) adding 80% ethanol with the volume 10 times that of the mint medicinal material into the filter residue d, and performing reflux extraction for 1h to obtain filtrate e and filter residue f;
and combining the filtrate a, the filtrate c and the filtrate e, and concentrating under reduced pressure to obtain the target mint fluid extract.
8. The compound rehabilitation new liquid mouthwash according to claim 1, wherein the mixed fluid extract filtrate is obtained by dissolving the mixed fluid extract in 75% ethanol, adding activated carbon for decolorization, and filtering while hot to obtain the target compound mixed fluid extract filtrate.
9. The preparation method of the compound rehabilitation new liquid mouthwash as claimed in any one of claims 1 to 8, wherein the compound rehabilitation new liquid mouthwash is prepared by mixing and stirring the mixed fluid extract filtrate and the rehabilitation new liquid uniformly according to a formula ratio.
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