CN106074305B - A kind of Noni fruit toothpaste and preparation method thereof with oral mucosa protective effect - Google Patents
A kind of Noni fruit toothpaste and preparation method thereof with oral mucosa protective effect Download PDFInfo
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
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- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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Abstract
The invention belongs to daily necessities fields, and in particular to a kind of Noni fruit toothpaste and preparation method thereof with oral mucosa protective effect.Noni fruit toothpaste provided by the invention with oral mucosa protective effect includes glucityl-Benexate Hydrochloride; glucityl-the Benexate Hydrochloride includes Noni fruit mixture and glucose group-beta-cyclodextrin, and the Noni fruit mixture is made of Noni extract, ethyl cellulose and Macrogol 4000.Noni fruit toothpaste provided by the invention with oral mucosa protective effect has significant bactericidal effect, can effectively reduce the feeling of pain of canker sore patient, shorten the healing time of canker sore, has significant protective effect to oral mucosa.And the Noni fruit toothpaste with oral mucosa protective effect provided by the invention has that moisture retention is good, it is high to stablize, and is a kind of ideal toothpaste.
Description
Technical field
The invention belongs to daily necessities fields, and in particular to a kind of Noni fruit toothpaste with oral mucosa protective effect and its
Preparation method.
Background technique
Toothpaste is the articles for daily use for cleaning tooth, protecting oral hygiene health.It is improved on the basis of tooth powder
It is formed, the tooth powder of early stage using calcium carbonate as rubbing agent and using soap as surfactant by forming.With science and technology
Development, toothpaste industry are also rapidly developed, and the development and application of new rubbing agent, thickener and surfactant makes tooth
Cream product constantly upgrades.
Currently, there is various toothpaste on the market, such as: it is toothpaste with fluoride, Chinese herbal toothpaste, inflammation-diminishing toothpaste, hypo-allergenic
Toothpaste and de-sludging whitening toothpaste etc..Toothpaste with fluoride is that suitable fluoride is added in toothpaste, can increase oral cavity partial
Fluorine forms strong protective layer in dental surface, to reduce the generation of saprodontia, and fluorine can also improve the anti-corruption of tooth
Erosion ability inhibits the growth and breeding of cariogenic bacterium, can preferably take care of one's teeth.But long-term Excess free enthalpy fluorine can cause body
Slow poisoning, influence the sclerous tissues of human body, including tooth, bone, some other soft tissue also had damage, while can also draw
Play den tal fluorosis and fluorosis of bone.
Chinese herbal toothpaste is that certain Chinese herbal medicines are added on the basis of ordinary toothpaste, with clearing heat and detoxicating, anti-inflammation hemostasia
Effect, to alleviate gingivitis have certain booster action.But since Chinese herbal medicine onset time is long, content is more, cause to imitate
Fruit is unobvious.Allergy-free toothpaste is that the desensitization ingredient such as potassium nitrate or strontium chloride is added in toothpaste, is had centainly to hypersensitive dentin
Relaxation effect, but potassium nitrate or strontium chloride are harmful to the human body, and are unfavorable for being used for a long time.Therefore, it researches and develops out and cleans
The problem of significant effect, highly-safe toothpaste are still current urgent need to resolve.
Chinese patent CN103417402B discloses a kind of Bactericidal azulene toothpaste, and the Bactericidal azulene toothpaste is by camomile
Ring, aluminium hydroxide, lauroyl both sexes base PG- acetate sodium phosphate, guar gum, sorb alcohol and water composition.The Bactericidal azulene
The advantages of toothpaste has foaming abundancy, sterilizing power strong, energy total care oral cavity, protects oral cavity and dental health, is that one kind meets
The sterilization toothpaste that modern requires.
Chinese patent CN103417400B discloses a kind of toothpaste containing vinegar, and the toothpaste containing vinegar is by glacial acetic acid, calcium carbonate, the moon
Osmanthus acyl both sexes base PG- acetate sodium phosphate, hydroxyethyl cellulose, sorb alcohol and water composition.The toothpaste containing vinegar has anti-inflammatory, takes off
It is quick, eliminate bad breath, the multi-efficiencies such as removing smoke spots, can total care oral cavity, protect oral cavity and dental health.
Chinese patent application 201510711524.6 discloses a kind of chitin tooth-caring toothpaste, the chitin tooth-caring toothpaste
Mainly by chitin, sorbierite liquid glucose, silica, lauryl sodium sulfate, sodium carboxymethylcellulose, deionized water, saccharin
Sodium, menthol, cloves, nipalgin rouge composition, the chitin tooth-caring toothpaste being prepared are removed with ordinary toothpaste cleaning oral cavity
Outside function, anti-treating dental ulcer, swelling and aching of gum, bleeding and other effects are had more ,-OH and NH is wherein contained in chitin molecule2+Polarity
Group can effectively inhibit the breeding of oral cavity harmful bacteria, be proliferated the growth of beneficial bacterium, improve internal environment of oral cavity, and chitin is exclusive
Trophic factors and function factor, have very strong biological compatibility and film forming ability, effective protection gum and the flank of tooth are not invaded
Erosion, protects oral cavity comprehensively.
However, the current toothpaste disadvantage that there is also dehydrations during storage is very fast, moisture-retaining capacity is low and stability is poor,
It is not able to satisfy the demand of modern still.
Summary of the invention
In order to solve the problems, such as that toothpaste exists during storage in the prior art, the purpose of the present invention is to provide one kind
Noni fruit toothpaste and preparation method thereof with oral mucosa protective effect, to solve the above problems.It is provided by the invention to have
The Noni fruit toothpaste of oral mucosa protective effect has significant protective effect to oral mucosa, and the Noni fruit toothpaste also has
There are moisture retention and frost resistance good, highly-safe, the high advantage of stability is a kind of ideal health type toothpaste.
The present invention provides a kind of Noni fruit toothpaste with oral mucosa protective effect, and the Noni fruit toothpaste includes Portugal
Glycosyl-beta-cyclodexterin inclusion compound, the glucityl-Benexate Hydrochloride include Noni fruit mixture and glucityl-β-ring paste
Essence, the Noni fruit mixture are made of Noni extract, ethyl cellulose and Macrogol 4000.
Further, additive amount of the glucityl-Benexate Hydrochloride in Noni fruit toothpaste is 1-15%, described
Glucityl-Benexate Hydrochloride preferred additive amount in Noni fruit toothpaste is 10%.
Further, the glucityl-Benexate Hydrochloride the preparation method comprises the following steps:
S1 cleans fresh Noni fruit, slice, and placing under conditions of temperature is 35-45 DEG C dry, pulverize 80-100 mesh
Sieve, obtains fine powder；The 6-8 times of volume fraction that above-mentioned fine powder total weight is added into fine powder is the ethanol solution of 55-65%, ultrasonic wave
25-35min is extracted, filtering obtains filtrate I；Then the second that 6-8 times of volume fraction of above-mentioned filter residue is 65-75% is added into filter residue
Alcoholic solution, ultrasonic wave extraction 20-30min, filtering, filtrate II；Merging filtrate, the recycling ethyl alcohol and dense under the conditions of temperature is 60 DEG C
Contracting, obtains Noni extract；
The obtained Noni extract of step S1 is uniformly mixed by S2 with ethyl cellulose and Macrogol 4000, obtains promise
Beautiful fruit mixture；
Water is added toward glucose group-beta-cyclodextrin in S3, is configured to glucose group-beta-cyclodextrin saturated aqueous solution；
The glucose group-beta-cyclodextrin saturated aqueous solution that step S3 is obtained is added in the Noni fruit mixture that step S2 is obtained by S4
In, 2-5h is stirred under conditions of temperature is 35-60 DEG C, is filtered, filter residue is dry under the conditions of 60 DEG C, 80 meshes are crossed, through P2O5
It is dry, obtain glucityl-Benexate Hydrochloride.
Further, Noni extract and ethyl cellulose and Macrogol 4000 2- in mass ratio in the step S2
4:1-3:3-5 is mixed；Noni fruit mixture and glucose group-beta-cyclodextrin 1:2-6 in mass ratio are carried out in the step S4
Mixing.
Further, Noni extract and ethyl cellulose and Macrogol 4000 in mass ratio 3 in the step S2:
2:4 is mixed；Noni fruit mixture is mixed with glucose group-beta-cyclodextrin 1:5 in mass ratio in the step S4.
Further, the Noni fruit toothpaste further includes following components:
40-60% calcium carbonate, 18-40% moisturizer, 4-8% adhesive, 2-4% sodium lauryl sulfate, 0.1-0.4% sugar
Smart sodium, 0.8-1.5% essence, 0.1-0.5% sorbic acid and 1-2% deionized water.
Further, the Noni fruit toothpaste further includes following components:
47.3% calcium carbonate, 30% moisturizer, 6% adhesive, 3% sodium lauryl sulfate, 0.2% saccharin sodium, 1.2% perfume
Essence, 0.3% sorbic acid and 2% deionized water.
Further, the moisturizer is by sorbierite, polyethylene glycol and chitosan oligosaccharide by weight 2-4:1-3:0.5-1 group
At；Described adhesive is made of sodium cellulose glycolate and lauryl glucoside by weight 4-6:1-3.
Further, the moisturizer is made of sorbierite, polyethylene glycol and chitosan oligosaccharide by weight 3:2:0.8；It is described
Adhesive is made of sodium cellulose glycolate and lauryl glucoside by weight 5:2.
In addition, the present invention also provides a kind of preparation method of Noni fruit toothpaste with oral mucosa protective effect, packet
Include following steps:
S1 is by calcium carbonate, moisturizer, adhesive, sodium lauryl sulfate, saccharin sodium, sorbic acid and deionized water in vacuum degree
To stir evenly under conditions of -0.08Mpa~0.10Mpa, mixture is obtained；
S2 essence and glucityl-Benexate Hydrochloride is added in the mixture that step S1 is obtained, be in vacuum degree-
Stirred evenly under conditions of 0.08Mpa~0.10Mpa to get.
The glucityl that the present invention uses-beta-cyclodextrin inclusion compound Noni fruit mixture is added in toothpaste, can effectively increase
The solubility of strong Noni extract, improves the bioavilability and stability of Noni extract.It is found through experiment that the present invention
The Noni fruit toothpaste with oral mucosa protective effect provided has significant bactericidal effect, to the sterilizing rate of Escherichia coli
Greater than 99.08%, 99.10% is greater than to the sterilizing rate of staphylococcus aureus, the sterilizing rate of Candida albicans is greater than
99.12%, 99.16% is greater than to the sterilizing rate of Streptococcus mutans, 98.04% is greater than to the sterilizing rate of porphyromonas gingivalis.
Noni fruit toothpaste provided by the invention with oral mucosa protective effect reads Escherichia coli, staphylococcus aureus, white
Coccus, Streptococcus mutans and porphyromonas gingivalis have significant bactericidal effect, are cured to mucous membrane of mouth, recurrent oral ulceration
It closes, inhibits plaque, mitigates gingivitis with preferable protection and therapeutic effect.
Further, it is found through experiment that, the Noni fruit toothpaste provided by the invention with oral mucosa protective effect can be with
Significantly (P < 0.05) reduces the feeling of pain of canker sore patient, shortens the ulcer time of canker sore patient, to canker sore
There is more significant protective effect with significant therapeutic effect, while to oral cavity.
Further, the moisturizing provided by the invention being made of sorbierite, polyethylene glycol and chitosan oligosaccharide by certain weight ratio
Agent has significant moistening effect, and chitosan oligosaccharide can solve due to sorbierite water content height and toothpaste is caused to stablize lacking for difference
It falls into.It is found through experiment that the Noni fruit toothpaste provided by the invention with oral mucosa protective effect is 20 DEG C in temperature, it is relatively wet
For under conditions of 54%, fluid loss when 48h illustrates provided by the invention by sorbierite, polyethylene glycol and shell degree less than 5.8%
Oligosaccharides mutually coordinated can be play a part of to enhance moisturizing by the moisturizer of certain weight ratio composition.
Further, provided by the invention to be made of by constant weight sodium cellulose glycolate and lauryl glucoside
Adhesive has the advantages that adhesiveness is strong and stability is high, and lauryl glucoside can be with effective solution hydroxylmethyl cellulose
Water outlet, anti-thick, lotion matt appearance, the defect for viscous mouth of brushing teeth easily occur in the storage process of toothpaste for plain sodium.It is sent out through test
Existing, the viscosity of the Noni fruit toothpaste provided by the invention with oral mucosa protective effect is smaller with the change rate of time,
At 90 days, viscosity be greater than 13Pas, illustrate it is provided by the invention by sodium cellulose glycolate and lauryl glucoside by one
The adhesive interaction for determining weight composition plays a part of to enhance the viscosity and stability of toothpaste, can effectively extend toothpaste
Shelf-life.
Compared with prior art, the Noni fruit toothpaste provided by the invention with oral mucosa protective effect has following excellent
Gesture:
(1) the Noni fruit toothpaste provided by the invention with oral mucosa protective effect has significant bactericidal effect, can
Effectively to reduce the feeling of pain of canker sore patient, shorten the healing time of canker sore, there is significant protection to oral cavity
Effect；
(2) the Noni fruit toothpaste provided by the invention with oral mucosa protective effect has moisture retention and frost resistance good,
Highly-safe, the high advantage of stability is a kind of ideal health type toothpaste.
Specific embodiment
The following describes the present invention further through the description of specific embodiments, but it is to limit of the invention that this, which is not,
System, those skilled in the art's basic thought according to the present invention can make various modifications or improvements, but without departing from this
The basic thought of invention, is all within the scope of the present invention.
Embodiment 1, a kind of preparation of glucityl-Benexate Hydrochloride
S1 cleans fresh Noni fruit, slice, and placing under conditions of temperature is 35 DEG C dry, pulverize 80 meshes, obtains carefully
Powder；The ethanol solution that 6 times of volume fractions of above-mentioned fine powder total weight are 55%, ultrasonic wave extraction 25min, mistake are added into fine powder
Filter, obtains filtrate I；Then the ethanol solution that 6 times of volume fractions of above-mentioned filter residue are 65%, ultrasonic wave extraction are added into filter residue
20min, filtering, filtrate II；Merging filtrate recycles ethyl alcohol and is concentrated under the conditions of temperature is 60 DEG C, obtains Noni extract；
The obtained Noni extract of step S1 is uniformly mixed by S2 with ethyl cellulose and Macrogol 4000, the promise
Beautiful berry extract is mixed with ethyl cellulose and Macrogol 4000 2:1:5 in mass ratio, obtains Noni fruit mixture；
Water is added toward glucose group-beta-cyclodextrin in S3, is configured to glucose group-beta-cyclodextrin saturated aqueous solution；
The glucose group-beta-cyclodextrin saturated aqueous solution that step S3 is obtained is added in the Noni fruit mixture that step S2 is obtained by S4
In, Noni fruit mixture is mixed with glucose group-beta-cyclodextrin 1:4 in mass ratio in the step S4, is in temperature
3h is stirred under conditions of 35 DEG C, is filtered, filter residue is dry under the conditions of 60 DEG C, 80 meshes are crossed, through P2O5It is dry, obtain glucityl-β-
Cyclodextrin inclusion compound.
Embodiment 2, a kind of preparation of glucityl-Benexate Hydrochloride
S1 cleans fresh Noni fruit, slice, and placing, which dry, pulverize under conditions of temperature is 40 DEG C, sieves with 100 mesh sieve, and obtains carefully
Powder；The ethanol solution that 8 times of volume fractions of above-mentioned fine powder total weight are 60%, ultrasonic wave extraction 30min, mistake are added into fine powder
Filter, obtains filtrate I；Then the ethanol solution that 8 times of volume fractions of above-mentioned filter residue are 70%, ultrasonic wave extraction are added into filter residue
25min, filtering, filtrate II；Merging filtrate recycles ethyl alcohol and is concentrated under the conditions of temperature is 60 DEG C, obtains Noni extract；
The obtained Noni extract of step S1 is uniformly mixed by S2 with ethyl cellulose and Macrogol 4000, the promise
Beautiful berry extract is mixed with ethyl cellulose and Macrogol 4000 3:2:4 in mass ratio, obtains Noni fruit mixture；
Water is added toward glucose group-beta-cyclodextrin in S3, is configured to glucose group-beta-cyclodextrin saturated aqueous solution；
The glucose group-beta-cyclodextrin saturated aqueous solution that step S3 is obtained is added in the Noni fruit mixture that step S2 is obtained by S4
In, the Noni fruit mixture is mixed with glucose group-beta-cyclodextrin 1:5 in mass ratio, under conditions of temperature is 55 DEG C
4h is stirred, filtering is dry under the conditions of 60 DEG C by filter residue, 80 meshes is crossed, through P2O5It is dry, obtain glucityl-beta-cyclodextrin inclusion compound
Object.
Embodiment 3, a kind of Noni fruit toothpaste with oral mucosa protective effect
The Noni fruit toothpaste with oral mucosa protective effect is composed of the following components:
6% glucityl-Benexate Hydrochloride, 55.6% calcium carbonate, 22% moisturizer, 8% adhesive, 4% lauryl alcohol
Sodium sulphate, 0.4% saccharin sodium, 1.5% essence, 0.5% sorbic acid and 2% deionized water；The moisturizer is by sorbierite, poly- second
Two pure and mild chitosan oligosaccharides are formed by weight 2:3:1；Described adhesive is by sodium cellulose glycolate and lauryl glucoside by weight
Amount is formed than 4:3.
Preparation method:
S1 is by calcium carbonate, moisturizer, adhesive, sodium lauryl sulfate, saccharin sodium, sorbic acid and deionized water in vacuum degree
To stir evenly under conditions of -0.08Mpa, mixture is obtained；
S2 essence and glucityl-Benexate Hydrochloride is added in the mixture that step S1 is obtained, be in vacuum degree-
Stirred evenly under conditions of 0.08Mpa to get.
Embodiment 4, a kind of Noni fruit toothpaste with oral mucosa protective effect
The Noni fruit toothpaste with oral mucosa protective effect is composed of the following components:
10% glucityl-Benexate Hydrochloride, 47.3% calcium carbonate, 30% moisturizer, 6% adhesive, 3% lauryl alcohol
Sodium sulphate, 0.2% saccharin sodium, 1.2% essence, 0.3% sorbic acid and 2% deionized water；The moisturizer is by sorbierite, poly- second
Two pure and mild chitosan oligosaccharides are formed by weight 3:2:0.8；Described adhesive is pressed by sodium cellulose glycolate and lauryl glucoside
Weight ratio 5:2 composition.
Preparation method is similar to Example 3.
Embodiment 5, a kind of Noni fruit toothpaste with oral mucosa protective effect
The Noni fruit toothpaste with oral mucosa protective effect is composed of the following components:
15% glucityl-Benexate Hydrochloride, 40.8% calcium carbonate, 36% moisturizer, 4% adhesive, 2% lauryl alcohol
Sodium sulphate, 0.2% saccharin sodium, 0.8% essence, 0.2% sorbic acid and 1% deionized water；The moisturizer is by sorbierite, poly- second
Two pure and mild chitosan oligosaccharides are formed by weight 4:1:0.5；Described adhesive is pressed by sodium cellulose glycolate and lauryl glucoside
Weight ratio 6:1 composition.
Preparation method is similar to Example 3.
Comparative example 1, a kind of Noni fruit toothpaste with oral mucosa protective effect
The Noni fruit toothpaste with oral mucosa protective effect is composed of the following components:
10% glucityl-Benexate Hydrochloride, 47.3% calcium carbonate, 30% moisturizer, 6% adhesive, 3% lauryl alcohol
Sodium sulphate, 0.2% saccharin sodium, 1.2% essence, 0.3% sorbic acid and 2% deionized water；The moisturizer is by sorbierite and gathers
Ethylene glycol is formed by weight 1:1；Described adhesive is by sodium cellulose glycolate and lauryl glucoside by weight 5:2 group
At.
Preparation method is similar to Example 3.
Difference with embodiment 4 is that the moisturizer is made of sorbierite and polyethylene glycol by weight 1:1.
Comparative example 2, a kind of Noni fruit toothpaste with oral mucosa protective effect
The Noni fruit toothpaste with oral mucosa protective effect is composed of the following components:
10% glucityl-Benexate Hydrochloride, 47.3% calcium carbonate, 30% moisturizer, 6% adhesive, 3% lauryl alcohol
Sodium sulphate, 0.2% saccharin sodium, 1.2% essence, 0.3% sorbic acid and 2% deionized water；The moisturizer is by sorbierite, poly- second
Two pure and mild chitosan oligosaccharides are formed by weight 1:1:1；Described adhesive is by sodium cellulose glycolate and lauryl glucoside by weight
Amount is formed than 5:2.
Preparation method is similar to Example 3.
Difference with embodiment 4 is that the moisturizer is by sorbierite, polyethylene glycol and chitosan oligosaccharide by weight 1:1:1
Composition.Comparative example 3, a kind of Noni fruit toothpaste with oral mucosa protective effect
The Noni fruit toothpaste with oral mucosa protective effect is composed of the following components:
10% glucityl-Benexate Hydrochloride, 47.3% calcium carbonate, 30% moisturizer, 6% adhesive, 3% lauryl alcohol
Sodium sulphate, 0.2% saccharin sodium, 1.2% essence, 0.3% sorbic acid and 2% deionized water；The moisturizer is by sorbierite, poly- second
Two pure and mild chitosan oligosaccharides are formed by weight 3:2:0.8；Described adhesive is sodium cellulose glycolate.
Preparation method is similar to Example 3.
Difference with embodiment 4 is that described adhesive is sodium cellulose glycolate.
Comparative example 4, a kind of Noni fruit toothpaste with oral mucosa protective effect
The Noni fruit toothpaste with oral mucosa protective effect is composed of the following components:
10% glucityl-Benexate Hydrochloride, 47.3% calcium carbonate, 30% moisturizer, 6% adhesive, 3% lauryl alcohol
Sodium sulphate, 0.2% saccharin sodium, 1.2% essence, 0.3% sorbic acid and 2% deionized water；The moisturizer is by sorbierite, poly- second
Two pure and mild chitosan oligosaccharides are formed by weight 3:2:0.8；Described adhesive is pressed by sodium cellulose glycolate and lauryl glucoside
Weight ratio 1:1 composition.
Preparation method is similar to Example 3.
Difference with embodiment 4 is, described adhesive by sodium cellulose glycolate and lauryl glucoside by weight
It is formed than 1:1.
Test example one, the sterilization test of Noni fruit toothpaste with oral mucosa protective effect
1, test material: the Noni fruit with oral mucosa protective effect prepared by embodiment 1, embodiment 2 and embodiment 3
Toothpaste.
2, test method: with reference to the measurement embodiment of method as defined in GB15979-2002 appendix C 3 to Escherichia coli, golden yellow
Color staphylococcus, Candida albicans, Streptococcus mutans and porphyromonas gingivalis bactericidal effect.
3, test result:
Test result is as shown in table 1.
Table 1 has the bactericidal effect of the Noni fruit toothpaste of oral mucosa protective effect
As shown in Table 1, the Noni fruit toothpaste provided by the invention with oral mucosa protective effect is to Escherichia coli, golden yellow
Color staphylococcus, Candida albicans, Streptococcus mutans and porphyromonas gingivalis have bactericidal effect, kill to Escherichia coli
Bacterium rate is greater than 99.08%, is greater than 98.24% to the sterilizing rate of staphylococcus aureus, is greater than to the sterilizing rate of Candida albicans
99.12%, 99.16% is greater than to the sterilizing rate of Streptococcus mutans, 98.04% is greater than to the sterilizing rate of porphyromonas gingivalis.
Noni fruit toothpaste provided by the invention with oral mucosa protective effect heals to mucous membrane of mouth, recurrent oral ulceration, suppression
Plaque processed mitigates gingivitis and has significant protection and therapeutic effect.
The clinical test of test example two, the Noni fruit toothpaste with oral mucosa protective effect to canker sore
1, test material: the Noni fruit toothpaste with oral mucosa protective effect prepared by embodiment 4.
2, subjects: selection 20-65 year old recurrent aphthous ulcer (RAU) patient 80, be randomly divided into test group with
Control group, every group each 40.
3, testing standard: subject is to meet to be included in and the healthy adult male and women of exclusion criteria.
3.1, be included in standard: whole body health in order, has RAU morbidity history but without whole body system disease；Can read,
Understand informed consent form and be ready to sign above, can be recorded according to test requirements document during test and participates in inspection at any time；Mouthful
At least one intracavitary canker sore and ulcer time of origin is less than 48h；Allergy will not be occurred to toothpaste and its ingredient；Do not make
With other treatment stomatocace medicine；The habit for not using other oral cleaning measures in addition to toothbrush, such as dental floss and gargled
Water, chew gum etc.；Other similar experimental study is not participated in simultaneously.
3.2, exclusion criteria: heavy recurrent aphthous ulcer, Behcet's disease；General disease background such as anaemia, digestibility are burst
Ulcer, clone's disease, acute infectious diseases, autoimmune disease etc.；Analgesic or treatment canker sore medicine are used in for 24 hours
Object；Antibiotic, anti-inflammatory drug are used in 1 month, whole body uses corticosteroid, immunosuppressor in 3 months；Smoke in 3 months,
Wine-head；Tumor patient；There are allergies to oral health care product or its ingredient；Women in the gestational period and nursing period.
4, evaluation index:
4.1, average ulcerative stage (day, D): evaluation period ulcer duration summation is divided by ulcer sum.
4.2, pain index (dividing, P): using the daily pain scores of Visual analogue scale (VAS) record ulcerative stage.VAS
Indicate the straight line using 10cm, 0 end of straight line indicates " painless ", and the end 10cm indicates " most violent pain ".Subject is according to pain
The level of sensitivity of pain is different, keeps a record in the corresponding scale of straight line, 1 time a day.
Evaluation index classification: D1: average ulcerative stage shortens (t is examined, P < 0.05)；D0: average ulcerative stage object variation (t inspection
It tests, P > 0.05)；P1: pain index reduces (t is examined, P < 0.05)；P0: pain index is unchanged (t is examined, P > 0.05).It comments
Price card is quasi-: effective (D1P1)；Effectively (D1P0Or D0P1)；(D in vain0P0)。
5, test method:
It teaches patient and records pain index, issue " canker sore record sheet ", while recording subject's telephone number, issue
Everyone a set of toothpaste, toothbrush, three before the meal 10min toothpaste is applied to affected part, fed again after Su Kou after 5min.Morning and evening 2 times daily,
It is brushed teeth with sent out toothpaste according to oneself traditional approach.Call-on back by phone then is carried out to subject daily, understands ulcer development, oral cavity
After ulcer healing, carries out examination of mouth and recycle " canker sore record sheet ", test is completed using double-blind study.
6, test result:
Test result is as shown in table 2 and table 3.
2 pain index test data of table
It as shown in Table 2, can be significant using the Noni fruit toothpaste provided by the invention with oral mucosa protective effect
(P < 0.05) reduces the feeling of pain of canker sore patient, has significant treatment to canker sore.
3 healing test data of table
It as shown in Table 3, can be significant using the Noni fruit toothpaste provided by the invention with oral mucosa protective effect
(P < 0.05) shortens the ulcer time of canker sore patient, has significant treatment to canker sore.
The moisture retention test of test example three, Noni fruit toothpaste with oral mucosa protective effect
1, test material: prepared by embodiment 3, embodiment 4, embodiment 5, comparative example 1 and comparative example 2 has oral mucosa
The Noni fruit toothpaste of protective effect.
2, test method: the lotion of identical weight is weighed respectively, is put into same containers, lotion and air contact area are made
It is equal, it is 20 DEG C in temperature, under the same terms that relative humidity is 54%, with the fluid loss of weight method measurement each sample.Same
Under the conditions of sample, test measurement three times, is averaged in parallel.Wherein: fluid loss=(sample-dehydration sample/sample) × 100%.
3, test result:
Test result is as shown in table 4.
Table 4 has the fluid loss measurement of the Noni fruit toothpaste of oral mucosa protective effect
As shown in Table 4, the Noni fruit toothpaste provided by the invention with oral mucosa protective effect is 20 DEG C in temperature, phase
Under conditions of being 54% to humidity, fluid loss when 48h is less than 5.8%, and prepared by comparative example 1 and comparative example 2 has oral cavity
The Noni fruit toothpaste of mucosa is 20 DEG C in temperature, and under conditions of relative humidity is 54%, fluid loss when 48h is greater than
8.8%, illustrate it is provided by the invention can phase by the moisturizer that certain weight ratio forms by sorbierite, polyethylene glycol and chitosan oligosaccharide
Mutually coordinate to play a part of to enhance moisturizing.
The viscosity test of test example four, Noni fruit toothpaste with oral mucosa protective effect
1, test material: prepared by embodiment 3, embodiment 4, embodiment 5, comparative example 3 and comparative example 4 has oral mucosa
The Noni fruit toothpaste of protective effect.
2, test method: use rotary viscosimeter, temperature be 28 DEG C under conditions of measurement sample in 90 days
Viscosity.
3, test result:
Test result is as shown in table 5.
5 toothpaste viscosity of table changes with time
As shown in Table 5, the viscosity of the Noni fruit toothpaste with oral mucosa protective effect of 1-3 of embodiment of the present invention preparation
As the change rate of time is smaller, at 90 days, viscosity was greater than 13Pas, and prepared by comparative example 3 and comparative example 4 has
The viscosity of the Noni fruit toothpaste of oral mucosa protective effect is larger with the change rate of time, at 90 days, viscosity be less than in
9Pas illustrates the adhesive provided by the invention being made of sodium cellulose glycolate and lauryl glucoside by constant weight
Interaction plays a part of to enhance the viscosity and stability of toothpaste, can effectively extend the shelf-life of toothpaste.
Claims (6)
1. a kind of Noni fruit toothpaste with oral mucosa protective effect, which is characterized in that the Noni fruit toothpaste includes glucose
Group-beta-cyclodextrin inclusion compound, the glucityl-Benexate Hydrochloride include Noni fruit mixture and glucose group-beta-cyclodextrin,
The Noni fruit mixture is made of Noni extract, ethyl cellulose and Macrogol 4000, the glucityl-β-ring paste
Additive amount of the inclusion compounds in Noni fruit toothpaste is 1-15%；
Glucityl-the Benexate Hydrochloride the preparation method comprises the following steps:
S1 cleans fresh Noni fruit, slice, and placing under conditions of temperature is 35-45 DEG C dry, pulverize 80-100 mesh, obtains
Fine powder；The 6-8 times of volume fraction that above-mentioned fine powder total weight is added into fine powder is the ethanol solution of 55-65%, ultrasonic wave extraction
25-35min, filtering, obtains filtrate I；Then it is molten that the ethyl alcohol that 6-8 times of volume fraction of above-mentioned filter residue is 65-75% is added into filter residue
Liquid, ultrasonic wave extraction 20-30min, filtering, filtrate II；Merging filtrate recycles ethyl alcohol under the conditions of temperature is 60 DEG C and filter is concentrated
Liquid obtains Noni extract；
The obtained Noni extract of step S1 is uniformly mixed by S2 with ethyl cellulose and Macrogol 4000, obtains Noni fruit
Mixture；
Water is added toward glucose group-beta-cyclodextrin in S3, is configured to glucose group-beta-cyclodextrin saturated aqueous solution；
The Noni fruit mixture that step S2 is obtained is added in the glucose group-beta-cyclodextrin saturated aqueous solution that step S3 is obtained S4,
2-5h is stirred under conditions of temperature is 35-60 DEG C, is filtered, filter residue is dry under the conditions of 60 DEG C, 80 meshes are crossed, through P2O5It is dry
It is dry, obtain glucityl-Benexate Hydrochloride；
The Noni fruit toothpaste further includes component:
40-60% calcium carbonate, 18-40% moisturizer, 4-8% adhesive, 2-4% sodium lauryl sulfate, 0.1-0.4% saccharin
Sodium, 0.8-1.5% essence, 0.1-0.5% sorbic acid and 1-2% deionized water；The moisturizer by sorbierite, polyethylene glycol and
Chitosan oligosaccharide is formed by weight 2-4:1-3:0.5-1；Described adhesive is pressed by sodium cellulose glycolate and lauryl glucoside
Weight ratio 4-6:1-3 composition.
2. as described in claim 1 with the Noni fruit toothpaste of oral mucosa protective effect, which is characterized in that the step S2
Middle Noni extract is mixed with ethyl cellulose and Macrogol 4000 2-4:1-3:3-5 in mass ratio；The step
Noni fruit mixture is mixed with glucose group-beta-cyclodextrin 1:2-6 in mass ratio in S4.
3. as claimed in claim 2 with the Noni fruit toothpaste of oral mucosa protective effect, which is characterized in that the step S2
Middle Noni extract is mixed with ethyl cellulose and Macrogol 4000 3:2:4 in mass ratio；Promise in the step S4
Beautiful fruit mixture is mixed with glucose group-beta-cyclodextrin 1:5 in mass ratio.
4. as described in claim 1 with the Noni fruit toothpaste of oral mucosa protective effect, which is characterized in that the Noni fruit
Toothpaste further includes following components:
47.3% calcium carbonate, 30% moisturizer, 6% adhesive, 3% sodium lauryl sulfate, 0.2% saccharin sodium, 1.2% essence,
0.3% sorbic acid and 2% deionized water.
5. the Noni fruit toothpaste as described in claim 1 or 4 with oral mucosa protective effect, which is characterized in that the guarantor
Humectant is made of sorbierite, polyethylene glycol and chitosan oligosaccharide by weight 3:2:0.8；Described adhesive by sodium cellulose glycolate and
Lauryl glucoside is formed by weight 5:2.
6. a kind of preparation method of the Noni fruit toothpaste a method as claimed in any one of claims 1 to 5 with oral mucosa protective effect,
Characterized by comprising the following steps:
S1 by calcium carbonate, moisturizer, adhesive, sodium lauryl sulfate, saccharin sodium, sorbic acid and deionized water vacuum degree be-
It is stirred evenly under conditions of 0.08Mpa~0.10Mpa, obtains mixture；
S2 essence and glucityl-Benexate Hydrochloride is added in the mixture that step S1 is obtained, be in vacuum degree-
Stirred evenly under conditions of 0.08Mpa~0.10Mpa to get.
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| CN1859852A (en) * | 2003-09-26 | 2006-11-08 | 诺丽公司 | Morinda citrifolia-based oral care compositions and methods |
| US20090016972A1 (en) * | 2005-11-25 | 2009-01-15 | Tamazi Omarovich Manasherov | Oral cavity care curative and prophylactic composition |
| CN104739726A (en) * | 2015-03-30 | 2015-07-01 | 美晨集团股份有限公司 | Traditional Chinese medicine toothpaste and preparation method thereof |
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| CN1859852A (en) * | 2003-09-26 | 2006-11-08 | 诺丽公司 | Morinda citrifolia-based oral care compositions and methods |
| US20090016972A1 (en) * | 2005-11-25 | 2009-01-15 | Tamazi Omarovich Manasherov | Oral cavity care curative and prophylactic composition |
| CN104739726A (en) * | 2015-03-30 | 2015-07-01 | 美晨集团股份有限公司 | Traditional Chinese medicine toothpaste and preparation method thereof |
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