CN107349171A - A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing - Google Patents

A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing Download PDF

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CN107349171A
CN107349171A CN201710622171.1A CN201710622171A CN107349171A CN 107349171 A CN107349171 A CN 107349171A CN 201710622171 A CN201710622171 A CN 201710622171A CN 107349171 A CN107349171 A CN 107349171A
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mouthwash
water
sterilization
accelerating
extract
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CN107349171B (en
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沈平凡
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Anhui Silver Lithium Biotechnology Development Co Ltd
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Anhui Silver Lithium Biotechnology Development Co Ltd
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Abstract

The present invention provides a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing, and in parts by weight, the preparing raw material of the mouthwash includes:Xylitol 15, ethanol 17, citric acid 0.1 3, green-tea extract 18, nutgall extractive 0.1 8, Honegsukle flower P.E 0.1 4, menthol 0.1 4, qualities of stevia extract 0.1 4, calcium chloride 0.1 4, honey 0.1 1.5, potassium sorbate 0.01 2.8, caramel colorant 03, vitamin C 0 3.5, vitamin B12 0.1 5, modified hanfangchin A 1 10, Nano Silver 0.0001 0.01, water 40 100.

Description

A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing
Technical field
The present invention relates to oral health care field, especially a kind of effectively antibacterial, sterilization and acceleration canker sore healing Mouthwash.
Technical background
Daily oral health care is for preventing and controlling mouth disease (carious tooth, gingivitis, the periodontal of bacterial plaque correlation Disease) have the function that it is important.The use of the bacterium that effective chemicals suppresses the formation of bacterial plaque or kills in bacterial plaque is control bacterium One effective way of spot.But conventional chemicals can not only result in the potential danger of drug resistance, due also to oral cavity is Into a big import of human body, therefore it is not that what antiseptic can be present in mouthwash.
It is a kind of common ulcerative damages illness for betiding mucous membrane of mouth meanwhile canker sore is commonly called as " aphtha ", it is more The positions such as lip inner side, tongue, tongue abdomen, cheek mucous membrane, vestibular ditch, soft palate are seen, the mucous membrane at these positions lacks keratinization layer or angle Change poor.Tongue ulcer, which refers to, betides tongue, the canker sore of tongue belly position.Sharp ache when canker sore is broken out, it is local to burn Pain is obvious, and severe patient can also influence diet, speak, and very big inconvenience is caused to daily life;Can concurrently halitosis, chronic pharyngitis, just The constitutional symptoms such as secret, headache, dizzy, nauseous, weak, irritated, heating, enlargement of lymph nodes, canker sore be it is a variety of because The result of plain comprehensive function.
For the above situation, the present invention provides a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing.
The content of the invention
The present invention provides a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing, in parts by weight, institute The preparing raw material for stating mouthwash includes:
As one embodiment of the present invention, in parts by weight, the preparing raw material of the mouthwash includes:
As one embodiment of the present invention, in parts by weight, the preparing raw material of the mouthwash includes:
As one embodiment of the present invention, the preparation method of the modified hanfangchin A is as follows:
A. under ice-water bath, 2.09mmol hanfangchin As are dissolved in 55mL dichloromethane, after being dispersed with stirring, dropwise Add 14.6mmol 1mol/L BBr3Solution;
B. after being added dropwise to complete, after the solution of generation is stirred at room temperature 24 hours, 30mL deionized water is added, it is described to go The temperature of ionized water is 0 DEG C;
C. with water layer in dichloromethane extraction three times step b, merge organic layer salt water washing, done with anhydrous sodium sulfate It is dry, filter, be concentrated in vacuo, obtain crude product, crude product obtains sterling through column chromatography separating purification.
As one embodiment of the present invention, the preparing raw material of the mouthwash also includes hanfangchin B.
As one embodiment of the present invention, the preparation method of the green-tea extract is as follows:
1) 1 part of fresh Rizhao Green Tea is taken, is crushed to 50 mesh, 30 parts of distilled water and 1 part of vitamin C is added, mixes To mixture;
2) said mixture is placed in Ultrasound Instrument, by the effect of ultrasonic wave, obtains green-tea extract.
As one embodiment of the present invention, the preparation method of the nutgall extractive is as follows:
(1) Chinese gall is crushed, deionized water immersion, water-bath, shaking, filters off filter residue, repeat aforesaid operations, merge filter Liquid, add activated carbon decolorizing, filter, filtrate is concentrated to give Chinese gall water extract;
(2) Chinese gall water extract and amelogenin are mixed, after stirring, obtains nutgall extractive.
As one embodiment of the present invention, the preparation method of the Honegsukle flower P.E is as follows:
1) extracting honeysuckle medicinal material, alcohol reflux extraction, filtration, merging filtrate, be concentrated under reduced pressure recovery ethanol, obtains concentrate;
2) step 1) concentrate is diluted with water to equivalent to 2-5 times medicinal material weight, filtering, and filtrate regulation pH is 2-6, is added on Adsorbed in the macroporous resin column pre-processed, first eluted, discarded with 2-4BV pure water with 1-3BV/h flow velocity, then with 1- 3BV/h flow velocity with 2-4BV 30%-50% ethanol and 2-4BV 60%-80% ethanol elution, collects ethanol elution respectively Liquid;
3) combining step 2) ethanol eluate, concentrate, dry, obtain Honegsukle flower P.E.
As one embodiment of the present invention, the preparation method of the qualities of stevia extract is as follows:
S01 takes STEVIA REBAUDIANA coarse powder, by solid-liquid ratio 1:10 (g/mL) plus water, 70 DEG C of extraction 1h, repeat extraction 2 times after filtering, Merging filtrate, make extract solution mass concentration be 1g crude drugs/10mL extract solutions its decompression volume concentration half, obtain dark brown liquid Body, as STEVIA REBAUDIANA aqueous extract;
S02 accurately weighs 1.0g cyclodextrin, is dissolved with the acetums of 100mL 1%, obtains 1% cyclodextrin acetum;
S03 measures stevia rebaudiana water extract 100mL, adds cyclodextrin acetum 50mL, stirs 5min, 40 DEG C of standings of water-bath 4 hours, decompression was filtered, and 100mL, as qualities of stevia extract are settled to after filtrate cooling.
As one embodiment of the present invention, the parts by weight of the hanfangchin B are 0.01 part.
Embodiment
Participate in the election of the detailed description of the invention below for being preferable to carry out method and including embodiment this hair can be more easily understood Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with art of the present invention The identical implication that technical staff is generally understood that.When contradiction be present, the definition in this specification is defined.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements Thing, step, method, product or device are not necessarily limited to those key elements, but can include not expressly listed other key elements or Such a composition, step, method, product or the intrinsic key element of device.
Conjunction " Consists of " excludes any key element do not pointed out, step or component.If be used in claim, this Phrase will make claim be closed, it is not included the material in addition to the material of those descriptions, but relative normal Except rule impurity.When being rather than immediately following in the clause that phrase " Consists of " appears in claim main body after theme, It is only limited to the key element described in the clause;Other key elements are not excluded outside the claim as entirety.
Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit During the Range Representation that choosing value limits, this, which is appreciated that, specifically discloses by any range limit or preferred value and any scope All scopes that any pairing of lower limit or preferred value is formed, regardless of whether the scope separately discloses.For example, when open During scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to 5 ", " 1 to 3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end Value and all integers and fraction within the range.
Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " any It is a kind of " refer to that the item that describes thereafter or event may or may not occur, and the description include situation that event occurs and The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, and it is specific to represent that the present invention is not limited to this Quantity, include the part of the amendment of the acceptable change without cause related basic function close to the quantity.Phase Answer, modify a numerical value with " about ", " about " etc., mean that the invention is not restricted to the exact numerical.It is approximate in some examples Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, scope limits can be with Combine and/or exchange, these scopes include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article " one kind " before key element of the present invention or component and "one" to key element or the quantitative requirement of component (i.e. occurrence number) unrestriction.Therefore "one" or " one kind " should be read as including one or at least one, and odd number The key element or component of form also include plural form, unless the obvious purport of the quantity refers to singulative.
" polymer " means by the polymerizable compound prepared by the monomer that polymerize identical or different type.Generic term " polymer " includes term " homopolymer ", " copolymer ", " terpolymer " and " EVA ".
" EVA " means the polymer prepared by polymerizeing at least two different monomers.Generic term " EVA " includes (its is general with term " terpolymer " for term " copolymer " (its typically to refer to the polymer prepared by two kinds of different monomers) To refer to the polymer prepared by three kinds of different monomers).It also includes the polymerization for planting monomer by polymerization four or more to manufacture Thing." blend " means that two or more polymer mixes the polymerization to be formed by physics or chemical method jointly Thing.
The present invention provides a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing, in parts by weight, institute The preparing raw material for stating mouthwash includes:
Xylitol:Xylitol originates in Finland, is extracted from the plant materials such as silver birch, Oak Tree, corncob, bagasse A kind of natural sweetener out, alias pentitol.Heretofore described xylitol is bought from Shanghai Aladdin biochemical technology stock Part Co., Ltd.
Ethanol:Alcohol is commonly called as, is a kind of organic matter, skeleton symbol CH3CH2OH or C2H5OH, molecular formula C2H6O, it is most normal The monohydric alcohol seen.Heretofore described ethanol is bought from Shanghai Aladdin biochemical technology limited company.
Citric acid:Citric acid is a kind of important organic acid, also known as citric acid, chemical name 2- hydroxy propanes -1,2,3- Tricarboxylic acids, clear crystal, often contain a molecular crystalline water, it is odorless, there is very strong tart flavour.In the present invention can the citric acid be one Water citric acid, and buy from Shanghai Aladdin biochemical technology limited company.
Green-tea extract:Green tea, refer to the young leaves or bud for taking tea tree.
Conventional tealeaves processing needs to be made by techniques such as fixing, shaping, drying respectively;Green tea is without hair Tea made of ferment, the natural materials of fresh leaf are remained, the Tea Polyphenols that contains, catechin, chlorophyll, caffeine, amino acid, dimension life The nutritional ingredients such as element are also more.
The preparation method of heretofore described green-tea extract is as follows:
1) 1 part of fresh Rizhao Green Tea is taken, is crushed to 50 mesh, 30 parts of distilled water and 1 part of vitamin C is added, mixes To mixture;
2) said mixture is placed in Ultrasound Instrument, by the effect of ultrasonic wave, obtains green-tea extract.
The 10 minutes ultrasonic wave extraction time, 40 DEG C of mixture temperature, ultrasonic power 260W.
The step of above-mentioned preparation method is without fixing, but use and add ascorbic method, it can not only ensure to live The effect of property enzyme, it can equally ensure Tea Polyphenols, catechin, chlorophyll, caffeine, amino acid, vitamins and other nutritious components Activity.The ascorbic content added in green tea does not influence ascorbic changes of contents in the preparing raw material of mouthwash.
Nutgall extractive:Chinese gall scientific name, also known as hundred worm storehouses, fermented Chinese gall herb and tea leaves, gall, it is the horned gall aphid of Homoptera aphid section Or melaphis peitan Tsai et Tang female adult parasitizes Anacardiaceae plant " Chinese sumac " and its belongs to the tender leaf or petiole of other plant together, stabs and generates one Kind cryptomere consor thing insect gall, gained after baked drying.
The preparation method of heretofore described nutgall extractive is as follows:(1) Chinese gall is crushed, deionized water immersion, Water-bath, shaking, filter residue is filtered off, repeat aforesaid operations, merging filtrate, add activated carbon decolorizing, filtered, filtrate is concentrated to give Chinese gall Water extract;
(2) Chinese gall water extract and amelogenin are mixed, after stirring, obtains nutgall extractive.
Honegsukle flower P.E:Honeysuckle, also known as honeysuckle (scientific name:Lonicera japonica)." honeysuckle " one is come from 《Compendium of Materia Medica》, because honeysuckle flowers are just opened as white, after switch to yellow, hence obtain one's name honeysuckle.Medicinal material honeysuckle is Caprifoliaceae Woodbine honeysuckle and congener dry flower or with the flower just opened.
Honeysuckle is cold in nature, sweet, enters lung, the heart, stomach, has the effect of clearing heat and detoxicating, anti-inflammatory, qi-restoratives treat wind, cures mainly swollen Completely descend disease, warm disease heating, the disease such as heat toxin large carbuncle and tumour.It is for dizziness, thirst, sweating and boring, enteritis, bacterium Dysentery, measles, pneumonia, encephalitis, epidemic meningitis, acute mastitis, septicemia, appendicitis, skin infection, ulcer boils, erysipelas, the parotid gland The illnesss such as inflammation, suppurative tonsillitis have certain curative effect.
The preparation method of heretofore described Honegsukle flower P.E is as follows:
1) extracting honeysuckle medicinal material, alcohol reflux extraction, filtration, merging filtrate, be concentrated under reduced pressure recovery ethanol, obtains concentrate;
2) step 1) concentrate is diluted with water to equivalent to 2-5 times medicinal material weight, filtering, and filtrate regulation pH is 2-6, is added on Adsorbed in the macroporous resin column pre-processed, first eluted, discarded with 2-4BV pure water with 1-3BV/h flow velocity, then with 1- 3BV/h flow velocity is respectively with 2-4BV30%-50% (volume fraction) ethanol and 2-4BV 60%-80% (volume fraction) second Alcohol elutes, and collects ethanol eluate;
3) combining step 2) ethanol eluate, concentrate, dry, obtain Honegsukle flower P.E.
Menthol:Organic compound, colorless needle crystals or granular.For the main component in peppermint and lavender essential oil, Exist with free and ester state.Heretofore described menthol is levorotatory menthol.
Heretofore described levorotatory menthol is bought from Shanghai Aladdin biochemical technology limited company.
Qualities of stevia extract:STEVIA REBAUDIANA is composite family, sweetleaf Chrysanthemum herbaceos perennial.Plant height 1-1.3 rice.Root tip fertilizer Greatly, 50-60 bars, it is long up to 25 centimetres.Stem is upright, and base portion tip lignifying, top is tender, dense short down, corolla base portion grey violet Red or white, top white.Achene is linear, slightly flat, brown, has pappus.The month at florescence 7-9, the fruiting period 9-11 months.STEVIA REBAUDIANA cured leaf In main component be steviol glycoside, not only sugariness is high, heat is low, also with certain pharmacological action.Stevia mainly has Treatment diabetes, control blood glucose, reduce blood pressure, be antitumor, anti diar rhea, improving immunity, the effect of enhancing metabolism etc., to control Obesity processed, regulation hydrochloric acid in gastric juice, recover neural fatigue and have the effect of fine, also have significant curative effect to heart disease, pediatric saprodontia etc., most It is important that it can eliminate the side effect of sucrose.
In the present invention, the preparation method of the qualities of stevia extract is as follows:
S01 takes STEVIA REBAUDIANA coarse powder, by solid-liquid ratio 1:10 (g/mL) plus water, 70 DEG C of extraction 1h, repeat extraction 2 times after filtering, Merging filtrate, make extract solution mass concentration be 1g crude drugs/10mL extract solutions its decompression volume concentration half, obtain dark brown liquid Body, as STEVIA REBAUDIANA aqueous extract;
S02 accurately weighs 1.0g cyclodextrin, is dissolved with 100mL 1% (mass fraction) acetum, obtains 1% cyclodextrin Acetum;
S03 measures stevia rebaudiana water extract 100mL, adds cyclodextrin acetum 50mL, stirs 5min, 40 DEG C of standings of water-bath 4 hours, decompression was filtered, and 100mL, as qualities of stevia extract are settled to after filtrate cooling.
Calcium chloride:Heretofore described calcium chloride is bought from Shanghai Aladdin biochemical technology limited company.
Honey:Heretofore described honey is sophorae honey.
Potassium sorbate:Heretofore described potassium sorbate is bought from Shanghai Aladdin biochemical technology limited company.
Caramel colorant:Also known as caramel colorant, also known as dark reddish brown, burnt sugar coloring, it is that glucide (such as maltose, sucrose, molasses, turns Change hydrolysate of sugar, lactose, malt syrup and starch etc.) the complicated bronzing that is dehydrated, decomposes and is polymerized at high temperature It is to apply wide half-natural food color or dark brown mixture, some of which are colloid aggregation.Institute in the present invention Caramel colorant purchase is stated from Zhengzhou Jun Kai chemical products Co., Ltd.
Vitamin C:Heretofore described vitamin C is bought from Shanghai Aladdin biochemical technology limited company.
Vitamin B12:Heretofore described vitamin B12 is bought from Shanghai Aladdin biochemical technology limited company.
Modified hanfangchin A:Hanfangchin A (Tetrandrine), alias Tet, tetrandrine, it is a kind of white The chemicals of color solid.Chemical name (S, S)-(+)-Tetrandrine, molecular formula C38H42N2O6, molecular weight 622.75, melt 217~218 DEG C of point.
The preparation method of heretofore described modified hanfangchin A is as follows:
A. under ice-water bath, 2.09mmol hanfangchin As are dissolved in 55mL dichloromethane, after being dispersed with stirring, dropwise Add 14.6mmol 1mol/LBBr3Solution;
B. after being added dropwise to complete, after the solution of generation is stirred at room temperature 24 hours, 30mL deionized water is added, it is described to go The temperature of ionized water is 0 DEG C;
C. with water layer in dichloromethane extraction three times step b, merge organic layer salt water washing, done with anhydrous sodium sulfate It is dry, filter, be concentrated in vacuo, obtain crude product, crude product obtains sterling through column chromatography separating purification.
As one embodiment of the present invention, the preparing raw material of heretofore described mouthwash also includes Stephania tetrandra second Element, and the parts by weight of the hanfangchin B are 0.01 part.
Nano Silver:Heretofore described Nano Silver is bought from Luoyang Ou Lun Environmental Protection Technology Co., Ltd, particle diameter 1-2nm.
As one embodiment of the present invention, in parts by weight, the preparing raw material of the mouthwash includes:
As the preferred embodiment of the present invention, in parts by weight, the preparing raw material of the mouthwash includes:
Another aspect of the invention provides the system of the effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing Preparation Method:Xylitol, citric acid and water are mixed, is stirred at 40 DEG C, obtains solution A;By ethanol, green-tea extract, Nutgall extractive, Honegsukle flower P.E, menthol and qualities of stevia extract mixing, are stirred at 40 DEG C, obtain molten Liquid B, then solution A and solution B are mixed under agitation, add surplus materials, continue to be stirred until homogeneous, be cooled to room temperature, i.e., Can.
Mechanism is explained:Conventional green tea needs to handle by fixing during processing, it is therefore an objective to is inner passivation reaction Enzyme, the present invention is not handled using fixing, but in the preparation process of green-tea extract, adds vitamin C material, not only can be with Temporarily suppress the effect of reaction enzymes, while the effect for nor affecting on Tea Polyphenols is put to good use.The extraction of heretofore described STEVIA REBAUDIANA Cyclodextrin is added in journey.Meanwhile amelogenin is with the addition of in heretofore described gallic extraction process, because five times Contain tannic acid material in seed extract, it can be with precipitating proteins, but it can form complex compound with metallics, so as to human body Certain injury is caused with tooth.The present invention adds amelogenin during preparation not only can temporarily avoid the danger of tannic acid Evil, while tannic acid can discharge albumen under the environment of alkalescence, also can be right so as to discharge effect of the amelogenin to human body The calcium discharged in tooth is adsorbed, and improves the rental of enamel.
Embodiment 1:Present embodiment provides a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing, In parts by weight, the preparing raw material of the mouthwash includes:
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 2., In parts by weight, the preparing raw material of the mouthwash includes:
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 3., In parts by weight, the preparing raw material of the mouthwash includes:
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 4., The preparation method of the modified hanfangchin A is as follows:
A. under ice-water bath, 2.09mmol hanfangchin As are dissolved in 55mL dichloromethane, after being dispersed with stirring, dropwise Add 14.6mmol 1mol/LBBr3Solution;
B. after being added dropwise to complete, after the solution of generation is stirred at room temperature 24 hours, 30mL deionized water is added, it is described to go The temperature of ionized water is 0 DEG C;
C. with water layer in dichloromethane extraction three times step b, merge organic layer salt water washing, done with anhydrous sodium sulfate It is dry, filter, be concentrated in vacuo, obtain crude product, crude product obtains sterling through column chromatography separating purification.
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 5., The preparing raw material of the mouthwash also includes hanfangchin B.
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 6., The preparation method of the green-tea extract is as follows:
1) 1 part of fresh Rizhao Green Tea is taken, is crushed to 50 mesh, 30 parts of distilled water and 1 part of vitamin C is added, mixes To mixture;
2) said mixture is placed in Ultrasound Instrument, by the effect of ultrasonic wave, obtains green-tea extract.
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 7., The preparation method of nutgall extractive described in embodiment is as follows:
(1) Chinese gall is crushed, deionized water immersion, water-bath, shaking, filters off filter residue, repeat aforesaid operations, merge filter Liquid, add activated carbon decolorizing, filter, filtrate is concentrated to give Chinese gall water extract;
(2) Chinese gall water extract and amelogenin are mixed, after stirring, obtains nutgall extractive.
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 8., The preparation method of the Honegsukle flower P.E is as follows:
1) extracting honeysuckle medicinal material, alcohol reflux extraction, filtration, merging filtrate, be concentrated under reduced pressure recovery ethanol, obtains concentrate;
2) step 1) concentrate is diluted with water to equivalent to 2-5 times medicinal material weight, filtering, and filtrate regulation pH is 2-6, is added on Adsorbed in the macroporous resin column pre-processed, first eluted, discarded with 2-4BV pure water with 1-3BV/h flow velocity, then with 1- 3BV/h flow velocity with 2-4BV30%-50% ethanol and 2-4BV60%-80% ethanol elution, collects ethanol eluate respectively;
3) combining step 2) ethanol eluate, concentrate, dry, obtain Honegsukle flower P.E.
A kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in the embodiment 1 of embodiment 9., The preparation method of the qualities of stevia extract is as follows:
S01 takes STEVIA REBAUDIANA coarse powder, by solid-liquid ratio 1:10 (g/mL) plus water, 70 DEG C of extraction 1h, repeat extraction 2 times after filtering, Merging filtrate, make extract solution mass concentration be 1g crude drugs/10mL extract solutions its decompression volume concentration half, obtain dark brown liquid Body, as STEVIA REBAUDIANA aqueous extract;
S02 accurately weighs 1.0g cyclodextrin, is dissolved with 100mL 1% (mass fraction) acetum, obtains 1% cyclodextrin Acetum;
S03 measures stevia rebaudiana water extract 100mL, adds cyclodextrin acetum 50mL, stirs 5min, 40 DEG C of standings of water-bath 4 hours, decompression was filtered, and 100mL, as qualities of stevia extract are settled to after filtrate cooling.
What a kind of effectively antibacterial, sterilization and acceleration canker sore described in the embodiment 5 of embodiment 10. were healed gargles Water, the parts by weight of the hanfangchin B are 0.01 part.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following examples are only used In the invention will be further described, it is impossible to be interpreted as limiting the scope of the invention, professional and technical personnel in the field Some the nonessential modifications and adaptations made according to the content of the invention described above, still fall within protection scope of the present invention.
In addition, if without other explanations, raw materials used is all commercially available.
Embodiment 1:The present embodiment provides a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing, according to Parts by weight meter, the preparing raw material of the mouthwash include:
Xylitol described in the present embodiment is bought from Shanghai Aladdin biochemical technology limited company.
Ethanol described in the present embodiment is bought from Shanghai Aladdin biochemical technology limited company.
In the present embodiment can the citric acid be Citric Acid Mono, and purchase have from Shanghai Aladdin biochemical technology share Limit company.
The preparation method of green-tea extract described in the present embodiment is as follows:
1) 1 part of fresh Rizhao Green Tea is taken, is crushed to 50 mesh, 30 parts of distilled water and 1 part of vitamin C is added, mixes To mixture;
2) said mixture is placed in Ultrasound Instrument, by the effect of ultrasonic wave, obtains green-tea extract.
The 10 minutes ultrasonic wave extraction time, 40 DEG C of mixture temperature, ultrasonic power 260W.
The preparation method of nutgall extractive described in the present embodiment is as follows:(1) by 1 parts by weight Chinese gall crush, go from Sub- water immersion, water-bath, shaking, filters off filter residue, repeats aforesaid operations, merging filtrate, add activated carbon decolorizing, filter, filtrate is dense Contract to obtain Chinese gall water extract;
(2) Chinese gall water extract and 0.1 parts by weight amelogenin are mixed, after stirring, obtains Chinese gall and carry Take thing.
The preparation method of Honegsukle flower P.E described in the present embodiment is as follows:
1) 5 parts by weight traditional Chinese medicine honeysuckles are taken, alcohol reflux extraction, filtration, merging filtrate, be concentrated under reduced pressure recovery ethanol, obtains Concentrate;
2) step 1) concentrate is diluted with water to equivalent to 2-5 times medicinal material weight, filtering, and filtrate regulation pH is 6, increases hole Adsorbed on resin column, first eluted, discarded, then 4BV is used with 1BV/h flow velocity respectively with 4BV pure water with 2BV/h flow velocity The ethanol elution of 30% ethanol and 3BV 60%, collect ethanol eluate;
3) combining step 2) ethanol eluate, concentrate, dry, obtain Honegsukle flower P.E.
Levorotatory menthol described in the present embodiment is bought from Shanghai Aladdin biochemical technology limited company.
In the present embodiment, the preparation method of the qualities of stevia extract is as follows:
S01 takes STEVIA REBAUDIANA coarse powder, by solid-liquid ratio 1:10 (g/mL) plus water, 70 DEG C of extraction 1h, repeat extraction 2 times after filtering, Merging filtrate, make extract solution mass concentration be 1g crude drugs/10mL extract solutions its decompression volume concentration half, obtain dark brown liquid Body, as STEVIA REBAUDIANA aqueous extract;
S02 accurately weighs 1.0g cyclodextrin, is dissolved with 100mL 1% (mass fraction) acetum, obtains 1% cyclodextrin Acetum;
S03 measures stevia rebaudiana water extract 100mL, adds cyclodextrin acetum 50mL, stirs 5min, 40 DEG C of standings of water-bath 4 hours, decompression was filtered, and 100mL, as qualities of stevia extract are settled to after filtrate cooling.
Calcium chloride described in the present embodiment is bought from Shanghai Aladdin biochemical technology limited company.
Honey described in the present embodiment is sophorae honey.
Potassium sorbate described in the present embodiment is bought from Shanghai Aladdin biochemical technology limited company.
Caramel colorant described in the present embodiment is bought from Zhengzhou Jun Kai chemical products Co., Ltd.
Vitamin C described in this implementation is bought from Shanghai Aladdin biochemical technology limited company.
Vitamin B12 described in the present embodiment is bought from Shanghai Aladdin biochemical technology limited company.
The preparation method of modified hanfangchin A is as follows described in the present embodiment:
A. under ice-water bath, 2.09mmol hanfangchin As are dissolved in 55mL dichloromethane, after being dispersed with stirring, dropwise Add 14.6mmol 1mol/LBBr3Solution;
B. after being added dropwise to complete, after the solution of generation is stirred at room temperature 24 hours, 30mL deionized water is added, it is described to go The temperature of ionized water is 0 DEG C;
C. with water layer in dichloromethane extraction three times step b, merge organic layer salt water washing, done with anhydrous sodium sulfate It is dry, filter, be concentrated in vacuo, obtain crude product, crude product obtains sterling through column chromatography separating purification.
The Environmental Protection Technology Co., Ltd of Luoyang Ou Lun described in the present embodiment, particle diameter 1-2nm.
The still further aspect of the present embodiment provides the mouthwash of effectively antibacterial, sterilization and acceleration the canker sore healing Preparation method:Xylitol, citric acid and water are mixed, is stirred at 40 DEG C, obtains solution A;Ethanol, green tea are extracted Thing, nutgall extractive, Honegsukle flower P.E, menthol and qualities of stevia extract mixing, are stirred at 40 DEG C, obtain Solution B, then solution A and solution B are mixed under agitation, add surplus materials, continue to be stirred until homogeneous, be cooled to room temperature, .
Embodiment 2:The present embodiment provides a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing, according to Parts by weight meter, the preparing raw material of the mouthwash include:
Embodiment 3:Difference with embodiment 1 is that the preparation method of the green-tea extract is as follows:
1) 1 part of fresh Rizhao Green Tea is taken, is crushed to 50 mesh, adds 30 parts of distilled water, mixing obtains mixture;
2) said mixture is placed in Ultrasound Instrument, by the effect of ultrasonic wave, obtains green-tea extract.
Embodiment 4:Difference with embodiment 1 is that the preparation method of the nutgall extractive is as follows:By gallnut extract It is broken, deionized water immersion, water-bath, shaking, filter residue is filtered off, repeat aforesaid operations, merging filtrate, add activated carbon decolorizing, filtered, Filtrate is concentrated to give nutgall extractive;
Embodiment 5:Difference with embodiment 1 is that the preparation method of the qualities of stevia extract is as follows:Take STEVIA REBAUDIANA thick Powder, by solid-liquid ratio 1:10 (g/mL) plus water, 70 DEG C of extraction 1h, repeat extraction 2 times, merging filtrate, by its decompression volume after filtering Concentration half makes extract solution mass concentration be 1g crude drugs/10mL extract solutions, obtains dark brown liquid, as qualities of stevia extract.
Embodiment 6:Difference with embodiment 1 is that the preparing raw material of the mouthwash is without modified hanfangchin A.
Embodiment 7:Difference with embodiment 1 is that the preparing raw material of the mouthwash is without the anti-second A prime of the Chinese.
Embodiment 8:Difference with embodiment 1 is that the preparing raw material of the mouthwash is without modified hanfangchin A and five Times seed extract.
Embodiment 9:Difference with embodiment 1 is that the preparing raw material of the mouthwash is without Nano Silver.
Embodiment 10:Difference with embodiment 1 is that the modified hanfangchin A is replaced by hanfangchin A.
Test:
(1) bacteriostasis:
Strain:Staphylococcus aureus, Escherichia coli, shigella dysenteriae, Pseudomonas aeruginosa, γ-streptococcus, Candida albicans;
Specific method of testing:The culture medium of each test bacterium is poured into culture dish, after culture medium completely solidification, with shifting Examination bacteria suspension is supplied to be smoothened with spreading rod in culture dish, take circular filter paper piece to dip mouthwash of the present invention needed for the absorption of liquid rifle, Each filter paper is uniformly placed on the culture medium for scribbling bacteria suspension, the sealing of culture dish sealed membrane, during one section of horizontal inversion culture Between after, taking-up with crossing method measure antibacterial circle diameter, and with the presence or absence of inhibition zone and inhibition zone size evaluation bactericidal activity.
Result of the test is as shown in table 1:
(2) clinical observation
Using opinion poll point system, the crowd for having canker sore to perplex for choosing 360 30-70 year age brackets is used as examination With object, 12 groups are arbitrarily divided into, the mouthwash prepared respectively with embodiment 1-10, usage time is four months, and one day with 2 It is secondary.
Test result counts:
Every using effect total score is 5 points:5 points are best result, represent fine, highly effective;4 points are preferable, hence it is evident that effect Fruit;3 points are to receive, effective;Less than 3 points is to no effect, it is impossible to receive.It is every average below.
As a result it is as shown in table 2 below:
Effect Alleviate bleeding gums Relief of caries Accelerate canker sore healing
Embodiment 1 4.8 4.7 4.6
Embodiment 2 4.7 4.6 4.6
Embodiment 3 3.5 3.8 3.2
Embodiment 4 3.1 3.2 2.9
Embodiment 5 4.1 4.2 4.0
Embodiment 6 1.8 2.1 1.7
Embodiment 7 2.8 3.0 2.7
Embodiment 8 1.6 1.8 1.5
Embodiment 9 2.1 2.5 2.2
Embodiment 10 2.0 2.3 2.0
(3) effect test of bacterial plaque is removed
1st, salivary flow cell research is carried out, wherein making bacterial plaque be grown on the surface of model, then with embodiment 1- 10 gargle and measures the reduction of bacterial plaque at water process surface.Under study for action, first by continuously by the medium of bacterial growth It is sprayed onto with pump on prism about 18 hours, bacterial plaque biofilm is formed on germanium prism.Then, in order to promote remove tooth bacterium Spot, with water process prism of gargling, i.e., mouthwash is sprayed onto a few minutes on prism with pump.With infrared spectrum (ATRFTIR) 3300, 1650th, 1545 and 1080cm-1The intensity of absorption bands at place calculates the index of bacterial plaque from following infrared spectrum:
Bacterial plaque is scored=abs3300+abs1650+abs1545+abs1080
Wherein abs is the absorption maximum at different wave numbers.Selected wave number represents salivary components and infrared-transparent germanium The infrared ray absorbing of bacterium on prism.Then it is the dental plaque index of the prism for water process of gargling is (only clear with salt solution with baseline The prism washed) compare, and it is recorded as the reduction percentage of bacterial plaque.
Secure data
Mouthwash of the present invention has preferable anti-inflammatory fungistatic effect after tested, but is necessarily noticed that whether in application process Safety, therefore, has made following security test.
1st, multiple (acute) Skin Irritation Test
Reference《Cosmetics safety technical specification (2015 editions)》Repeatedly (acute) Skin Irritation Test is carried out, is as a result proved: Gargle water security, non-stimulated.
2nd, mucomembranous irritant test
Mouthwash of the present invention is subjected to oral mucosa, gingival mucosa stimulation test to rabbit and doggie, as a result proved:This hair Bright mouthwash is non-stimulated to mucous membrane, pathologic lesion.
Experiment confirm mouthwash of the present invention be it is a kind of it is harmless, nontoxic, have no side effect, the thing that non-stimulated safety coefficient is big Product.
Foregoing example is merely illustrative, some features of the feature for explaining the disclosure.Appended claim It is intended to require the scope as wide as possible being contemplated that, and embodiments as presented herein is only according to all possible embodiment Combination selection embodiment explanation.Therefore, the purpose of applicant is appended claim not by the explanation present invention Feature example selectional restriction.And the progress in science and technology will not formed due to the inaccuracy of language performance and not The possible equivalent or son being presently considered are replaced, and these changes should also be interpreted by appended in the conceived case Claim covers.

Claims (10)

1. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing, it is characterised in that in parts by weight, institute The preparing raw material for stating mouthwash includes:
2. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that In parts by weight, the preparing raw material of the mouthwash includes:
3. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that In parts by weight, the preparing raw material of the mouthwash includes:
4. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that The preparation method of the modified hanfangchin A is as follows:
A. under ice-water bath, 2.09mmol hanfangchin As are dissolved in 55mL dichloromethane, after being dispersed with stirring, are added dropwise 14.6mmol 1mol/LBBr3Solution;
B. after being added dropwise to complete, after the solution of generation is stirred at room temperature 24 hours, 30mL deionized water, the deionization are added The temperature of water is 0 DEG C;
C. with water layer in dichloromethane extraction three times step b, organic layer salt water washing is merged, with anhydrous sodium sulfate drying, mistake Filter, it is concentrated in vacuo, obtains crude product, crude product obtains sterling through column chromatography separating purification.
5. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that The preparing raw material of the mouthwash also includes hanfangchin B.
6. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that The preparation method of the green-tea extract is as follows:
1) 1 part of fresh Rizhao Green Tea is taken, is crushed to 50 mesh, 30 parts of distilled water and 1 part of vitamin C is added, is mixed Compound;
2) said mixture is placed in Ultrasound Instrument, by the effect of ultrasonic wave, obtains green-tea extract.
7. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that The preparation method of the nutgall extractive is as follows:
(1) Chinese gall is crushed, deionized water immersion, water-bath, shaking, filters off filter residue, repeatedly aforesaid operations, merging filtrate, Add activated carbon decolorizing, filter, filtrate is concentrated to give Chinese gall water extract;
(2) Chinese gall water extract and amelogenin are mixed, after stirring, obtains nutgall extractive.
8. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that The preparation method of the Honegsukle flower P.E is as follows:
1) extracting honeysuckle medicinal material, alcohol reflux extraction, filtration, merging filtrate, be concentrated under reduced pressure recovery ethanol, obtains concentrate;
2) step 1) concentrate is diluted with water to equivalent to 2-5 times medicinal material weight, filtering, and filtrate regulation pH is 2-6, is added on pre- place Adsorbed in the macroporous resin column managed, first eluted, discarded with 2-4BV pure water with 1-3BV/h flow velocity, then with 1-3BV/ H flow velocity with 2-4BV30%-50% ethanol and 2-4BV60%-80% ethanol elution, collects ethanol eluate respectively;
3) combining step 2) ethanol eluate, concentrate, dry, obtain Honegsukle flower P.E.
9. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 1, it is characterised in that The preparation method of the qualities of stevia extract is as follows:
S01 takes STEVIA REBAUDIANA coarse powder, by solid-liquid ratio 1:10 add water, 70 DEG C of extraction 1h, extraction 2 times are repeated after filtering, merging filtrate will Its decompression volume concentration half makes extract solution mass concentration be 1g crude drugs/10mL extract solutions, obtains dark brown liquid, as STEVIA REBAUDIANA Aqueous extract;
S02 accurately weighs 1.0g cyclodextrin, is dissolved with the acetums of 100mL 1%, obtains 1% cyclodextrin acetum;
S03 measures stevia rebaudiana water extract 100mL, adds cyclodextrin acetum 50mL, stirs 5min, it is small that 40 DEG C of water-bath stands 4 When, decompression is filtered, and 100mL, as qualities of stevia extract are settled to after filtrate cooling.
10. a kind of effectively antibacterial, sterilization and the mouthwash for accelerating canker sore healing described in claim 5, it is characterised in that The parts by weight of the hanfangchin B are 0.01 part.
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CN108175736A (en) * 2018-01-22 2018-06-19 福建美菰林生物科技有限公司 Gargle and preparation method thereof
CN108186541A (en) * 2018-03-19 2018-06-22 纳诺神蜂(福建)个人护理用品有限公司 Multi-efficiency type mouthwash and preparation method thereof
CN110354018A (en) * 2019-07-29 2019-10-22 广西壮族自治区农业科学院 A kind of Tea Saponin mouthwash and preparation method thereof
CN112826923A (en) * 2021-01-21 2021-05-25 华熙生物科技股份有限公司 Composition for treating oral ulcer, oral ulcer membrane and preparation method thereof

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CN102579702A (en) * 2012-03-14 2012-07-18 山东赛克赛斯药业科技有限公司 Medicine for treating dental ulcer and preparation method thereof
CN103735473A (en) * 2013-12-04 2014-04-23 何小刚 Herbal mouthwash and preparation method thereof

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CN1823702A (en) * 2005-12-31 2006-08-30 升联国际生物科技股份有限公司 Oral cavity health protection composition and its preparation method
CN102579702A (en) * 2012-03-14 2012-07-18 山东赛克赛斯药业科技有限公司 Medicine for treating dental ulcer and preparation method thereof
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CN108175736A (en) * 2018-01-22 2018-06-19 福建美菰林生物科技有限公司 Gargle and preparation method thereof
CN108175736B (en) * 2018-01-22 2020-12-01 福建美菰林生物科技有限公司 Gargle and preparation method thereof
CN108186541A (en) * 2018-03-19 2018-06-22 纳诺神蜂(福建)个人护理用品有限公司 Multi-efficiency type mouthwash and preparation method thereof
CN110354018A (en) * 2019-07-29 2019-10-22 广西壮族自治区农业科学院 A kind of Tea Saponin mouthwash and preparation method thereof
CN112826923A (en) * 2021-01-21 2021-05-25 华熙生物科技股份有限公司 Composition for treating oral ulcer, oral ulcer membrane and preparation method thereof

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