CN109381350A - One kind toothpaste containing polygonum cuspidate and preparation method thereof - Google Patents
One kind toothpaste containing polygonum cuspidate and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- 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
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- 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
本发明属于日化用品领域，具体涉及一种含虎杖牙膏及其制备方法。本发明提供的含虎杖牙膏组分及重量百分比为虎杖提取物0.5％～8％，摩擦型二氧化硅15％～25％，增稠型二氧化硅3％～10％，甘油10％～18％，山梨糖醇液40％～52％，羧甲基纤维素钠1％～3％，十二烷基硫酸钠1.5％～3％，糖精钠0.1％～0.5％，苯甲酸钠0.2％～0.4％，薄荷脑0.3％～0.5％，柠檬酸0.2％～0.4％，去离子水余量。本发明制备的含虎杖牙膏性状均一透明，具有与人体唾液接近的pH，能保持蒽醌类和鞣质类活性成分不被氧化并保持较强的抑菌防龋功效，并且能美白牙齿、清新口气、提神醒脑。The invention belongs to the field of daily chemical products, in particular to a toothpaste containing Polygonum cuspidatum and a preparation method thereof. The components and weight percentages of the toothpaste containing Polygonum cuspidatum provided by the invention are: 0.5% to 8% of Polygonum cuspidatum extract, 15% to 25% of frictional silica, 3% to 10% of thickened silica, and 10% to 18% of glycerin. %, sorbitol solution 40%～52%, sodium carboxymethyl cellulose 1%～3%, sodium lauryl sulfate 1.5%～3%, sodium saccharin 0.1%～0.5%, sodium benzoate 0.2%～0.4 %, menthol 0.3%～0.5%, citric acid 0.2%～0.4%, balance of deionized water. The toothpaste containing Polygonum cuspidatum prepared by the invention has uniform and transparent properties, has a pH close to that of human saliva, can keep the active components of anthraquinones and tannins from being oxidized, maintains strong antibacterial and anti-caries effects, and can whiten teeth, refresh and refresh the teeth. Breathe, refresh your mind.
Description
Technical field
The invention belongs to daily chemical product fields, and in particular to one kind toothpaste containing polygonum cuspidate and preparation method thereof.
Background technique
Saprodontia is commonly called as decayed tooth, decayed tooth, is a kind of communicable disease of oral cavity common disease, Streptococcus mutans
(Streptococcus mutans) and two kinds of streptococcus mutans of Soxhlet streptococcus (Streptococcus sobrinus) are main
The pathogenic bacteria wanted.Pathogenic bacteria generate glucoinvertase (GTFs), and synthesize the glucose not soluble in water from sucrose, this makes
The surface of tooth can be securely attached to by obtaining bacterium, and promote the formation of plaque.Saprodontia can be with secondary pulpitis and the tip of a root
Zhou Yan, or even alveolar bone and inflammation of jaws can be caused.Saprodontia is such as not treated in time, and lesion continues to develop, and cavity is formed, eventually to tooth
Hat destroys completely, eventually leads to loss of tooth.
Many mothproof antibacterial toothpastes use fluoride as antipathogenic composition on the market, and this toothpaste with fluoride is for reducing saprodontia
Certain effect is truly had, but is appropriate only for promoting the use of in low fluorine area, suitable fluorine area and in dental caries hotspot, in high fluorine
Regional crowd and 6 years old or less children's use will lead to fluorine poisoning, and less serious case forms den tal fluorosis, and severe one leads to fluorosis of bone.In in recent years
Medicine effect toothpaste continues the antibacterial function of whitening and is favored by market, it is neat to form kind because the strong tooth of its natural component protects gum
Entirely, the functional toothpaste vdiverse in function for meeting various demands.
Polygonum cuspidatum Sieb. et Zucc has anti-infective, anti-inflammatory, anti-oxidant, antitumor, Metabolism regulation, Organoprotective, anti-fibrosis, resists and stop
Gram etc. extensive pharmacological action.The active constituent of Polygonum cuspidatum Sieb. et Zucc includes rheum emodin, Physcion, polygonin and resveratrol.
There is presently no functional toothpaste as active constituent of polygonum cuspidate or Gentrin Knotweed P.E is used alone, only contain polygonum cuspidate etc. it is a variety of in
Medicine collectively forms functional toothpaste prepared by active ingredient, such as Chinese patent CN106619156.Chinese patent
CN106619156 disclose it is a kind of following weight match substance made of toothpaste: calcium phosphate dibasic anhydrous 20~30%, hydroxyl
Apatite 1~5%, sorbierite 15~25%, glycerol 5~10%, sodium lauroyl sarcosine 1~3%, sodium alginate 1~2%,
Quadrafos 0.5~1.5%, xylitol 0.5~1%, menthol 0.5~1%, Radix Glycyrrhizae 1~5%, Asian puccoon 1~5%, blackberry lily 1
~3%, honeycomb 0.5~1.5%, polygonum cuspidate 0.5~1.5% and water 5.5~51.5%.Asian puccoon is its main antipathogenic composition, polygonum cuspidate
It is then preventing phlegm from forming and stopping coughing, analgesic effect.Chinese patent CN106619156 has the following disadvantages: (1) anhydrous phosphoric acid used in
Hydrogen calcium, hydroxyapatite, sodium lauroyl sarcosine, sodium alginate, Quadrafos are basic auxiliary, lead to that toothpaste finally is made
In alkalinity, the fungistatic effect of antipathogenic composition can be reduced；(2) pH of human saliva is 6.6~7.1, and alkaline toothpaste can destroy oral cavity
PH environment, change oral cavity flora structure and reduce have bactericidal effect lysozyme activity；(3) Anthraquinones etc. in toothpaste
Active constituent can reduce activity because of oxidation, reduce the bacteriostatic activity and effect of toothpaste；(4) contain 5 kinds of Chinese medicines such as Asian puccoon, polygonum cuspidate,
Decocting liquid extracting mode is taken, solvent polarity is big, and the lesser active constituent of polarity is caused not extract completely, can not will be in medicinal material
Effective active composition sufficiently extract, reduce medicinal material utilization rate.
Summary of the invention
In order to solve the problems in the existing technology, the purpose of the present invention is to provide one kind containing only a kind of Chinese medicine of polygonum cuspidate
Toothpaste and preparation method thereof.
A kind of toothpaste containing polygonum cuspidate, the toothpaste component and weight percent are as follows:
Gentrin Knotweed P.E 0.5%~8%, friction-type silica 1 5%~25%, thickening type silica 3%~
10%, glycerol 10%~18%, D-sorbitol solution 40%~52%, sodium carboxymethylcellulose 1%~3%, dodecyl sulphate
Sodium 1.5%~3%, saccharin sodium 0.1%~0.5%, sodium benzoate 0.2%~0.4%, menthol 0.3%~0.5%, lemon
Acid 0.2%~0.4%, deionized water surplus；
The extracting method of the Gentrin Knotweed P.E is polygonum cuspidate to be beaten powder after 60 DEG C or less drying, then extracted with ethyl alcohol, is mentioned
Take liquid drying to medicinal extract sample to get the Gentrin Knotweed P.E, in terms of medicinal material, the D-sorbitol solution is Gentrin Knotweed P.E weight
The aqueous solution of 69%~71% D-sorbite.
Further, the composition of the toothpaste are as follows: Gentrin Knotweed P.E 1%, friction-type silica 1 8%, thickening type dioxy
SiClx 7%, glycerol 15%, D-sorbitol solution 46%, sodium carboxymethylcellulose 2%, lauryl sodium sulfate 3%, saccharin sodium
0.3%, sodium benzoate 0.4%, menthol 0.4%, citric acid 0.3%, deionized water surplus.
Further, the weight percent of the citric acid is 0.3%~0.4%.
Further, the weight ratio of the friction-type silica and thickening type silica is (2~6): 1.
Further, the toothpaste also contains arginine, and arginine wt percentage is 0.1%~0.2%.
The present invention also provides a kind of preparation methods of toothpaste containing polygonum cuspidate, comprising the following steps:
(1) polygonum cuspidate beats powder after 60 DEG C or less drying, then is extracted with ethyl alcohol, and extracting solution drying is to medicinal extract sample to get polygonum cuspidate
Extract；
(2) Gentrin Knotweed P.E adds deionized water dissolving, removes insoluble matter, obtains Gentrin Knotweed P.E clear aqueous solution；
(3) D-sorbitol solution, glycerol, sodium benzoate, saccharin sodium, lemon is added in Xiang Suoshu Gentrin Knotweed P.E clear aqueous solution
Acid is uniformly mixed, obtains mixed liquor A；
(4) friction-type silica, thickening type silica, sodium carboxymethylcellulose, lauryl sodium sulfate are mixed
Uniformly, mixed powder B is obtained；
(5) mixed powder B is added in Xiang Suoshu mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) menthol is added in Xiang Suoshu mixing paste, deionized water is added to supply surplus, vacuum mixer is stirred until homogeneous
It is translucent to obtain the final product.
Further, step (1) polygonum cuspidate drying temperature is 40 DEG C~60 DEG C, and concentration of alcohol is 70wt%~80wt%.
Further, step (1) extracting method includes seepage pressure effects, refluxing extraction, ultrasonic extraction.
Further, extracting liquid volume and polygonum cuspidate weight ratio are 10:1~15:1, seepage pressure effects in the extracting method
When diacolation speed be 3~5mL/kg/min.
Further, step (2) deionized water is 1~3 times of Rhizoma Polygoni Cuspidati weight.
Further, the method that step (2) removes insoluble matter includes filtration method, centrifugal process, settled process, the centrifugal process
Centrifugal rotational speed is 1500r/min~2500r/min, and centrifugation time is 5min~15min.
Polygonum cuspidate is the dry rhizome and root of polygonaceae plant polygonum cuspidate.It is distributed Central China and south, originates in Jiangsu, Zhejiang, river
The ground such as west, Fujian, Shandong, Henan, Shaanxi, Hubei, Yunnan, Sichuan, Guizhou.Polygonum cuspidate has extensive pharmacological action, including anti-
Infection, anti-inflammatory, anti-oxidant, antitumor, Metabolism regulation, Organoprotective, anti-fibrosis, Hemorrhagic shock etc..
The cause pathogeny imcrobe infections main components such as polygonum cuspidate is antiviral, bacterium, fungi, helminth are rheum emodin, rheum emodin Portugal
Polyglycoside, polydatin, tannin.The ethanol extract of polygonum cuspidate shows stronger bacteriostasis within the scope of a certain concentration,
Two kinds of cariogenic streptococcus mutans of Streptococcus mutans and Streptococcus sobrinus are significantly inhibited
Effect, while having significant suppression to grignard streptococcus, Streptococcus sanguis, micrococcus scarlatinae, staphylococcus aureus, actinomyces
Production is used.Therefore, the toothpaste of the ethanol extract containing polygonum cuspidate has the effect of antibacterial preventing decayed tooth, and polygonum cuspidate is main antiseptic caries-preventing ingredient.
But the active constituent tannin and anthraquinone in polygonum cuspidate are oxidizable, and there are also thermal sensitivity and light sensitivity for polydatin, so that containing
The study on the stability of polygonum cuspidate toothpaste becomes important factor.
For the pH of toothpaste prepared by the present invention between 6~7, pH adjusting agent used is citric acid.Citric acid is in this hair
Play a key role in bright: (1) bacteriostatic active ingredients are rheum emodin, polydatin, tannin etc. in Gentrin Knotweed P.E, are contained
Phenolic hydroxyl group isoreactivity group, weak acid property retention active constituent have good inhibitory effect；(2) pH of human saliva is 6.6
~7.1, it is in neutrality or faintly acid, lemon acid for adjusting pH to 6~7 coincide substantially with the pH of human saliva, can have and keep oral cavity raw
PH environment is managed, guarantees the bioactivity of mucin in oral cavity, glutinous polysaccharide, ptyalin, lysozyme, immunoglobulin, especially
It can guarantee that lysozyme has good bactericidal effect (can be stabilized in acid medium, easy in inactivation in alkaline medium) in oral cavity；
(3) citric acid has antioxidation, avoids or reduces the Anthraquinones such as polydatin and tannin active component oxidation deterioration,
Bacteriostatic activity reduces.
Friction-type silica and thickening type silica are bought from DENTSIL company, wherein friction-type silica
Make rubbing agent, thickening type silica makees thickener.Friction-type silica frictional force is stronger, for removing tooth stain, whitening；Thickening
Type silica mainly plays thickening power, and the transparency that can not only improve toothpaste (connects with the index of refraction of friction-type silica
Closely), at the same can be reduced sodium carboxymethylcellulose it is filling when generate wire drawing phenomenon, be conducive to filling.
Menthol is aromatic, and menthol has effects that fresh breath, refreshes the mind.
Arginine can improve bitter drawback after corrigent saccharin sodium, further increase the compliance of toothpaste.
Compared with prior art, the beneficial effects of the present invention are:
(1) the preparation method mild condition of Gentrin Knotweed P.E and can effectively extract in polygonum cuspidate with antibacterial anticaries action work
Property ingredient, the utilization rate of medicinal material is high.
(2) polygonum cuspidate toothpaste prepared by the present invention has suitable pH value, close with human saliva pH, is able to maintain physiology of oral cavity
PH environment can guarantee that lysozyme has good bactericidal effect in oral cavity；In suitable weak acid property retention polygonum cuspidate Anthraquinones and
The molecular state of tannin active component keeps bacteriostatic activity not decline.
(3) citric acid have antioxidation, can guarantee the Anthraquinones such as polydatin and tannin active component not by
Oxidation, keeps the bacteriostatic activity of active constituent not reduce.
(4) friction-type silica and the collaboration of thickening type silica use, and can not only improve the transparency of toothpaste, make it
Character transparent and homogeneous；And it is avoided that generation wire drawing phenomenon when sodium carboxymethylcellulose is filling, be conducive to filling.
(5) arginine can improve bitter drawback after corrigent saccharin sodium, improve the compliance of polygonum cuspidate toothpaste.
Specific implementation method
The present invention is described in further details below by specific embodiment, keeps those skilled in the art better
Understand that the present invention, these embodiments are only used for the purpose of illustration, are in no way intended to limit protection scope of the present invention.
One, embodiment
Embodiment 1
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 0.5%, friction-type silica 1 8% increase
Thick type silica 3%, glycerol 13%, D-sorbitol solution 52%, sodium carboxymethylcellulose 1%, lauryl sodium sulfate
1.5%, saccharin sodium 0.1%, sodium benzoate 0.2%, menthol 0.3%, citric acid 0.2%, deionized water 10.2%.Polygonum cuspidate mentions
Take object weight in terms of medicinal material.
Preparation method:
(1) it takes 0.5 parts by weight polygonum cuspidate to beat powder after 60 DEG C of drying, then is extracted with 5 parts by weight 70wt% ethanol percolations, diacolation
Speed is 3ml/kg/min, and extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 0.5 parts by weight of deionized water to dissolve, and 1500r/min is centrifuged 15min, obtains polygonum cuspidate extraction
Object clear aqueous solution；
(3) 0.2 parts by weight sodium, 0.1 parts by weight saccharin sodium, 0.2 weight is added to Gentrin Knotweed P.E clear aqueous solution
Amount part citric acid sufficiently dissolve, then with 52 parts by weight D-sorbitol solutions, 13 parts by weight of glycerin, be uniformly mixed, obtain mixed liquor A；
(4) by 18 parts by weight of friction type silica, 3 parts by weight thickening type silica, 1 parts by weight carboxymethyl cellulose
Sodium, 1.5 parts by weight lauryl sodium sulfate are uniformly mixed, and obtain mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.3 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Embodiment 2
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 1%, friction-type silica 1 8%, thickening
Type silica 7%, glycerol 15%, D-sorbitol solution 46%, sodium carboxymethylcellulose 2%, lauryl sodium sulfate 3%, sugar
Smart sodium 0.3%, sodium benzoate 0.4%, menthol 0.4%, citric acid 0.3%, deionized water 6.6%.Gentrin Knotweed P.E weight
In terms of medicinal material.
Preparation method:
(1) it takes 1 parts by weight polygonum cuspidate to beat powder after 55 DEG C of drying, then is extracted with 12 parts by weight 70wt% alcohol refluxs, 80 DEG C
Flow back 45min, and extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 3 parts by weight of deionized water to dissolve, and filtering obtains Gentrin Knotweed P.E clear aqueous solution；
(3) 0.4 parts by weight sodium, 0.3 parts by weight saccharin sodium, 0.3 weight is added to Gentrin Knotweed P.E clear aqueous solution
Amount part citric acid sufficiently dissolve, then with 46 parts by weight D-sorbitol solutions, 15 parts by weight of glycerin, be uniformly mixed, obtain mixed liquor A；
(4) by 18 parts by weight of friction type silica, 7 parts by weight thickening type silica, 2 parts by weight carboxymethyl celluloses
Sodium, 3 parts by weight lauryl sodium sulfate are uniformly mixed, and obtain mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.4 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Embodiment 3
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 4%, friction-type silica 25%, thickening
Type silica 6%, glycerol 10%, D-sorbitol solution 40%, sodium carboxymethylcellulose 2.5%, lauryl sodium sulfate
2.2%, saccharin sodium 0.5%, sodium benzoate 0.2%, menthol 0.5%, citric acid 0.3%, arginine 0.1%, deionized water
8.7%.Gentrin Knotweed P.E weight is in terms of medicinal material.
Preparation method:
(1) it takes 4 parts by weight polygonum cuspidates to beat powder after 50 DEG C of drying, then is extracted with 60 parts by weight 80wt% EtOH Sonicates, ultrasound
30min, extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 6 parts by weight of deionized water to dissolve, and with multilayer filtered through gauze, obtains Gentrin Knotweed P.E clarification
Aqueous solution；
(3) 0.2 parts by weight sodium, 0.5 parts by weight saccharin sodium, 0.3 weight is added to Gentrin Knotweed P.E clear aqueous solution
Amount part citric acid, 0.1 parts by weight arginine sufficiently dissolve, then with 40 parts by weight D-sorbitol solutions, 10 parts by weight of glycerin, mixing is equal
It is even, obtain mixed liquor A；
(4) by 25 parts by weight of friction type silica, 6 parts by weight thickening type silica, 2.5 parts by weight carboxymethyl celluloses
Plain sodium, 2.2 parts by weight lauryl sodium sulfate are uniformly mixed, and obtain mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.5 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Embodiment 4
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 8%, friction-type silica 1 5%, thickening
Type silica 4%, glycerol 12%, D-sorbitol solution 43%, sodium carboxymethylcellulose 3%, lauryl sodium sulfate 2.3%,
Saccharin sodium 0.4%, sodium benzoate 0.3%, menthol 0.3%, citric acid 0.4%, deionized water 11.3%.Gentrin Knotweed P.E weight
Amount is in terms of medicinal material.
Preparation method:
(1) it takes 8 parts by weight polygonum cuspidates to beat powder after 40 DEG C of drying, then is extracted with 80 parts by weight 75wt% ethanol percolations, diacolation
Speed is 5ml/kg/min, and extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 8 parts by weight of deionized water to dissolve, and stands 12h, takes supernatant, it is clear to obtain Gentrin Knotweed P.E
Clear water solution；
(3) 0.3 parts by weight sodium, 0.4 parts by weight saccharin sodium, 0.4 weight is added to Gentrin Knotweed P.E clear aqueous solution
Amount part citric acid sufficiently dissolve, then with 43 parts by weight D-sorbitol solutions, 12 parts by weight of glycerin, be uniformly mixed, obtain mixed liquor A；
(4) by 15 parts by weight of friction type silica, 4 parts by weight thickening type silica, 3 parts by weight carboxymethyl celluloses
Sodium, 2.3 parts by weight lauryl sodium sulfate are uniformly mixed, and obtain mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.3 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Embodiment 5
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 2%, friction-type silica 20%, thickening
Type silica 1 0%, glycerol 18%, D-sorbitol solution 42%, sodium carboxymethylcellulose 1.5%, lauryl sodium sulfate
1.8%, saccharin sodium 0.2%, sodium benzoate 0.2%, menthol 0.4%, citric acid 0.2%, deionized water 3.7%.Polygonum cuspidate mentions
Take object weight in terms of medicinal material.
Preparation method:
(1) it takes 2 parts by weight polygonum cuspidates to beat powder after 50 DEG C of drying, then is extracted with 24 parts by weight 80wt% ethanol percolations, diacolation
Speed is 4ml/kg/min, and extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 2 parts by weight of deionized water to dissolve, and stands 12h, takes supernatant, it is clear to obtain Gentrin Knotweed P.E
Clear water solution；
(3) 0.2 parts by weight sodium, 0.2 parts by weight saccharin sodium, 0.2 weight is added to Gentrin Knotweed P.E clear aqueous solution
Amount part citric acid sufficiently dissolve, then with 42 parts by weight D-sorbitol solutions, 18 parts by weight of glycerin, be uniformly mixed, obtain mixed liquor A；
(4) 20 parts by weight of friction type silica, 10 parts by weight thickening type silica, 1.5 parts by weight carboxymethyls are fine
It is uniformly mixed to tie up plain sodium, 1.8 parts by weight lauryl sodium sulfate, obtains mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.4 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Two, comparative example
Comparative example 1
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 1%, friction-type silica 1 8%, thickening
Type silica 7%, glycerol 15%, D-sorbitol solution 46%, sodium carboxymethylcellulose 2%, lauryl sodium sulfate 3%, sugar
Smart sodium 0.3%, sodium benzoate 0.4%, menthol 0.4%, deionized water 6.9%.
Preparation method:
(1) it takes 1 parts by weight polygonum cuspidate to beat powder after 55 DEG C of drying, then is extracted with 12 parts by weight 70wt% alcohol refluxs, 80 DEG C
Flow back 45min, and extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 3 parts by weight of deionized water to dissolve, and filtering obtains Gentrin Knotweed P.E clear aqueous solution；
(3) sufficiently molten to 0.4 parts by weight sodium of Gentrin Knotweed P.E clear aqueous solution addition, 0.3 parts by weight saccharin sodium
Solution, then with 46 parts by weight D-sorbitol solutions, 15 parts by weight of glycerin, be uniformly mixed, obtain mixed liquor A；
(4) by 18 parts by weight of friction type silica, 7 parts by weight thickening type silica, 2 parts by weight carboxymethyl celluloses
Sodium, 3 parts by weight lauryl sodium sulfate are uniformly mixed, and obtain mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.4 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Comparative example 2
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 1%, friction-type silica 1 8%, thickening
Type silica 7%, glycerol 15%, D-sorbitol solution 46%, sodium carboxymethylcellulose 2%, lauryl sodium sulfate 3%, sugar
Smart sodium 0.3%, sodium benzoate 0.4%, menthol 0.4%, acetic acid 0.3%, deionized water 6.6%.
Preparation method:
(1) it takes 1 parts by weight polygonum cuspidate to beat powder after 55 DEG C of drying, then is extracted with 12 parts by weight 70wt% alcohol refluxs, 80 DEG C
Flow back 45min, and extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 3 parts by weight of deionized water to dissolve, and filtering obtains Gentrin Knotweed P.E clear aqueous solution；
(3) 0.4 parts by weight sodium, 0.3 parts by weight saccharin sodium, 0.3 weight is added to Gentrin Knotweed P.E clear aqueous solution
Amount part acetic acid sufficiently dissolve, then with 46 parts by weight D-sorbitol solutions, 15 parts by weight of glycerin, be uniformly mixed, obtain mixed liquor A；
(4) by 18 parts by weight of friction type silica, 7 parts by weight thickening type silica, 2 parts by weight carboxymethyl celluloses
Sodium, 3 parts by weight lauryl sodium sulfate are uniformly mixed, and obtain mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.4 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Comparative example 3
The component and weight percent of the toothpaste containing polygonum cuspidate are as follows: Gentrin Knotweed P.E 1%, friction-type silica 1 8%, glycerol
15%, D-sorbitol solution 46%, sodium carboxymethylcellulose 2%, lauryl sodium sulfate 3%, saccharin sodium 0.3%, sodium benzoate
0.4%, menthol 0.4%, citric acid 0.3%, deionized water 13.6%.
Preparation method:
(1) it takes 1 parts by weight polygonum cuspidate to beat powder after 55 DEG C of drying, then is extracted with 12 parts by weight 70wt% alcohol refluxs, 80 DEG C
Flow back 45min, and extracting solution drying is to medicinal extract sample to get Gentrin Knotweed P.E；
(2) Gentrin Knotweed P.E adds 3 parts by weight of deionized water to dissolve, and filtering obtains Gentrin Knotweed P.E clear aqueous solution；
(3) 0.4 parts by weight sodium, 0.3 parts by weight saccharin sodium, 0.3 weight is added to Gentrin Knotweed P.E clear aqueous solution
Amount part citric acid sufficiently dissolve, then with 46 parts by weight D-sorbitol solutions, 15 parts by weight of glycerin, be uniformly mixed, obtain mixed liquor A；
(4) by 18 parts by weight of friction type silica, 2 parts by weight sodium carboxymethylcelluloses, 3 parts by weight dodecyl sulphates
Sodium is uniformly mixed, and obtains mixed powder B；
(5) mixed powder B is added to mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) 0.4 parts by weight menthol is added into mixing paste, deionized water is added to supply surplus, vacuum mixer stirring
To uniformly it is translucent to obtain the final product.
Three, test example
1 Gentrin Knotweed P.E biocidal property of test example is investigated
1. test material: polygonum cuspidate percolate medicinal extract obtained by 70% ethanol percolation
2. subjects: streptococcus mutans CNCC32400
3. test method:
1) 0.201g polygonum cuspidate medicinal extract (being equivalent to crude drug amount 0.810g) plus water 2mL are taken, ultrasound is to evenly dispersed, and concentration is with life
Medicine is calculated as 405mg/mL, and 0.22 μm of filtering with microporous membrane is spare as positive control solution, takes 0.807g polygonum cuspidate medicinal extract (with medicinal material
It is calculated as 3.25g), add water 20mL, for ultrasound to evenly dispersed, concentration is calculated as 162.6mg/mL, 0.22 μm of miillpore filter mistake with crude drug
Filter, it is spare as experimental liquid；
2) 21 test tubes are taken, are respectively divided into three groups of parallel test groups, every group 7, for first group, number is respectively
1H1、2H1、3H1、4H1、5H1、N1、P1, wherein H1For first group of test group, by number from small to large, concentration then successively halves, N1
For first group of negative control group, P1For first group of positive controls, second group is numbered with third group same way；
3) it is separately added into 1mL culture medium into test group, is separately added into 0.5mL into negative control group, positive controls
Culture medium；
4) to 1H1、1H2、1H3In be separately added into 1mL experimental group medical fluid, mix, take respectively 1mL be added 2H1、2H2、2H3, mix
Respectively take 1mL that 3H is added after even1、3H2、3H3, same operation to 5H1、5H2、5H3, three test tubes discard 1mL respectively；
5) it is separately added into 0.5mL distilled water into negative control group, mixes, is separately added into 0.5mL in heliotropism control group
High concentration medical fluid mixes；
6) it is separately added into 20 μ L bacterium solutions into each test tube, mixes；
7) test tube is put into 150rpm in shaking table, 37 DEG C, for 24 hours, whether observation test tube has muddiness for culture.
3. experimental result: in terms of crude drug, concentration is in 5.08mg/mL~81.3mg/mL, compared with negative control group, bright
It is aobvious more limpid, it was demonstrated that in the concentration range, polygonum cuspidate extracting solution has significant fungistatic effect.Test example 2
The polygonum cuspidate toothpaste sample and 1~2 sample of comparative example for taking the embodiment of the present invention 1~5 to prepare carry out pH value measurement, and will
Embodiment and comparative example sample is placed 3 months under the conditions of 25 ± 2 DEG C, then using HPLC method measurement polydatin content and
It as a result see the table below using disk diffusion method according to inhibition zone size measurement bacteriostatic activity.
| pH | Inoxidizability | Antibacterial circle diameter (mm) | Character | |
| Embodiment 1 | 6.8 | Polydatin content is not remarkably decreased | 36.7 | It is transparent |
| Embodiment 2 | 6.7 | Polydatin content is not remarkably decreased | 38.7 | It is transparent |
| Embodiment 3 | 6.9 | Polydatin content is not remarkably decreased | 42.2 | It is transparent |
| Embodiment 4 | 6.5 | Polydatin content is not remarkably decreased | 46.3 | It is transparent |
| Embodiment 5 | 6.8 | Polydatin content is not remarkably decreased | 40.5 | It is transparent |
| Comparative example 1 | 7.2 | Polydatin content decline about 11% | 24.9 | It is transparent |
| Comparative example 2 | 6.8 | Polydatin content decline about 8% | 28.4 | It is transparent |
Test example 3
The polygonum cuspidate toothpaste sample and 3 sample of comparative example for taking the embodiment of the present invention 1~2 to prepare carry out examining for character and characteristic
It examines, as a result see the table below.
| Character | Wire drawing | |
| Embodiment 1 | It is transparent | Without wire drawing phenomenon |
| Embodiment 2 | It is transparent | Without wire drawing phenomenon |
| Comparative example 3 | Poor transparency | There are wire drawing phenomenons |
Claims (10)
1. a kind of toothpaste containing polygonum cuspidate, which is characterized in that the toothpaste component and weight percent are as follows:
Gentrin Knotweed P.E 0.5%~8%, friction-type silica 1 5%~25%, thickening type silica 3%~10% are sweet
Oil 10%~18%, D-sorbitol solution 40%~52%, sodium carboxymethylcellulose 1%~3%, lauryl sodium sulfate 1.5%
~3%, saccharin sodium 0.1%~0.5%, sodium benzoate 0.2%~0.4%, menthol 0.3%~0.5%, citric acid 0.2%
~0.4%, deionized water surplus；
The extracting method of the Gentrin Knotweed P.E is polygonum cuspidate to be beaten powder after 60 DEG C or less drying, then extracted with ethyl alcohol, extracting solution
Drying is to medicinal extract sample to get the Gentrin Knotweed P.E, and Gentrin Knotweed P.E weight is in terms of medicinal material；
The D-sorbitol solution is the aqueous solution of 69%~71% D-sorbite.
2. toothpaste as described in claim 1, which is characterized in that the weight percent of the citric acid is 0.3%~0.4%.
3. toothpaste as described in claim 1, which is characterized in that the weight of the friction-type silica and thickening type silica
Amount is than being (2~6): 1.
4. toothpaste as described in claim 1, which is characterized in that the toothpaste also contains arginine, the arginine wt hundred
Divide than being 0.1%~0.2%.
5. a kind of preparation method for preparing any toothpaste containing polygonum cuspidate of Claims 1 to 4, which is characterized in that including following step
It is rapid:
(1) polygonum cuspidate beats powder after 60 DEG C or less drying, then is extracted with ethyl alcohol, and extracting solution is dry to be extracted to medicinal extract sample to get polygonum cuspidate
Object；
(2) Gentrin Knotweed P.E adds deionized water dissolving, removes insoluble matter, obtains Gentrin Knotweed P.E clear aqueous solution；
(3) D-sorbitol solution, glycerol, sodium benzoate, saccharin sodium, citric acid is added in Xiang Suoshu Gentrin Knotweed P.E clear aqueous solution,
It is uniformly mixed, obtains mixed liquor A；
(4) friction-type silica, thickening type silica, sodium carboxymethylcellulose, lauryl sodium sulfate are uniformly mixed,
Obtain mixed powder B；
(5) mixed powder B is added in Xiang Suoshu mixed liquor A, vacuum mixer is stirred until homogeneous, and obtains mixing paste；
(6) menthol is added in Xiang Suoshu mixing paste, deionized water is added to supply surplus, vacuum mixer is stirred until homogeneous semi-transparent
It is bright to obtain the final product.
6. the preparation method of toothpaste as claimed in claim 5, which is characterized in that step (1) polygonum cuspidate drying temperature is 40 DEG C~60
DEG C, concentration of alcohol is 70wt%~80wt%.
7. the preparation method of toothpaste as claimed in claim 5, which is characterized in that step (1) extracting method includes seepage pressure effects, returns
Stream extraction, ultrasonic extraction.
8. the preparation method of toothpaste as claimed in claim 7, which is characterized in that extracting liquid volume and polygonum cuspidate in the extracting method
Weight ratio is 10:1~15:1, and diacolation speed is 3~5mL/kg/min.
9. the preparation method of toothpaste as claimed in claim 5, which is characterized in that step (2) deionized water is polygonum cuspidate medicine
1~3 times of material weight.
10. the preparation method of toothpaste as claimed in claim 5, which is characterized in that step (2) remove insoluble matter method include
The centrifugal rotational speed of filtration method, centrifugal process, settled process, the centrifugal process is 1500r/min~2500r/min, and centrifugation time is
5min~15min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110898108A (en) * | 2019-12-10 | 2020-03-24 | 柳州两面针股份有限公司 | Application of giant knotweed rhizome in preparing oral care product |
| WO2021195110A1 (en) * | 2020-03-24 | 2021-09-30 | Colgate-Palmolive Company | Improved methods for manufacturing arginine dentifrice |
| CN117731558A (en) * | 2023-12-11 | 2024-03-22 | 扬州完美日用品有限公司 | High-stability toothpaste and preparation method thereof |
| CN118161560A (en) * | 2024-03-01 | 2024-06-11 | 湖北中医药大学 | External powder for treating acute eczema and preparation method thereof |
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| CN1291471A (en) * | 2000-09-06 | 2001-04-18 | 江西江中制药技术中心 | Application of Chinese Medicine and tooth-paste containing it |
| CN101938978A (en) * | 2008-02-08 | 2011-01-05 | 高露洁-棕榄公司 | Oral care products and methods of use and manufacture thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1291471A (en) * | 2000-09-06 | 2001-04-18 | 江西江中制药技术中心 | Application of Chinese Medicine and tooth-paste containing it |
| CN101938978A (en) * | 2008-02-08 | 2011-01-05 | 高露洁-棕榄公司 | Oral care products and methods of use and manufacture thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110898108A (en) * | 2019-12-10 | 2020-03-24 | 柳州两面针股份有限公司 | Application of giant knotweed rhizome in preparing oral care product |
| WO2021195110A1 (en) * | 2020-03-24 | 2021-09-30 | Colgate-Palmolive Company | Improved methods for manufacturing arginine dentifrice |
| US20210308027A1 (en) * | 2020-03-24 | 2021-10-07 | Colgate-Palmolive Company | Methods for Manufacturing Arginine Dentifrice |
| CN115297933A (en) * | 2020-03-24 | 2022-11-04 | 高露洁-棕榄公司 | Improved method for making arginine dentifrice |
| US12370133B2 (en) * | 2020-03-24 | 2025-07-29 | Colgate-Palmolive Company | Methods for manufacturing arginine dentifrice |
| CN117731558A (en) * | 2023-12-11 | 2024-03-22 | 扬州完美日用品有限公司 | High-stability toothpaste and preparation method thereof |
| CN118161560A (en) * | 2024-03-01 | 2024-06-11 | 湖北中医药大学 | External powder for treating acute eczema and preparation method thereof |
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