CN108175737A - A kind of anti-calculus dentalis Chinese medicinal toothpaste and preparation method thereof - Google Patents
A kind of anti-calculus dentalis Chinese medicinal toothpaste and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
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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
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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Abstract
The invention belongs to technical field of toothpaste, and in particular to a kind of anti-calculus dentalis Chinese medicinal toothpaste and preparation method thereof.Toothpaste of the present invention includes bletilla striata extract, 5~8 parts of the Chinese medicine of pearl shell powder and borneol composition, 0.1~0.3 part of saccharin sodium, 0.05~0.1 part of tertiary sodium phosphate, 3~6 parts of glycerine, 40~60 parts of sorbierite, 0.2~0.9 part of titanium dioxide, 0.2~0.6 part of carragheen, 0.5~1 part of carboxymethyl cellulose, 10~15 parts of silicon 201A, 302 3~8 parts of silicon, 103 3~8 parts of silicon, 2~3 parts of lauryl sodium sulfate, 0.1~0.5 part of menthol, 0.01~0.2 part of menthyl lactate, 23 0.2~0.9 part of freshener WS, 0.05~0.2 part of methyl hydroxybenzoate, 15~23 parts of 0.05~0.2 part of ethylparaben and water.Toothpaste of the present invention can effectively inhibit plaque, slow down the formation of calculus dentalis, have the effect of anti-calculus dentalis.
Description
Technical field
The invention belongs to technical field of toothpaste, and in particular to a kind of anti-calculus dentalis Chinese medicinal toothpaste and preparation method thereof.
Background technology
Calculus dentalis is a kind of calcification for being deposited on facing or dummy surface or just in the bacterial plaque of calcification and soft dirt, by saliva
Calcium salt in liquid or level in gingival sulcus fluid gradually deposits, and is not easy to remove after formation.Two basic steps that calculus dentalis is formed are tooth bacterium
It the formation of spot biomembrane and mineralizes.The initial stage that calculus dentalis is formed is plaque, and initial sialoprotein or glycoprotein are adsorbed to
Facing forms one layer without structure, acellular dental cuticle, and main component is substantially similar to saliva, contains mucoprotein, sugar
Albumen, blood-group antigen and immunoglobulin, some of which ingredient can promote bacterium to stick refined surface, play the work(of receptor
Energy.Then, the substances such as the protein, polysaccharide, lipoteichoicacid that intraoral bacterium passes through its surface are attached on film successively,
Bacterium forms complicated flora, using 10~30 days, bacterial plaque mature reached by sticking and copolymerization interconnects, is proliferated
To peak.On bacterial plaque surface, because the cell that mineral mineralization, swill and the necrosis in saliva come off participates in, in bacterial plaque shape
Into 2~14 days can calcification, be hardened and form calculus.
Periodontal disease is that the mankind are distributed one of most wide disease.Its Etiological is local stimulation factor, and calculus dentalis is
Cause the main local factor of periodontosis.Calculus dentalis is widely present in population of China, to safeguard periodontal health, is advocated people and is determined
Phase cleans one's teeth.Cleaning oral cavity calculus dentalis mainly uses mechanical removal at present, but if without effective method after removing calculus dentalis
Inhibit the formation of calculus dentalis, then enamel can be easily damaged by the way of mechanical removal for a long time.Thus using chemistry route
Calculus dentalis is inhibited to become the research hotspot of medical circle of oral cavity.Toothpaste is that oral cleaning indispensable in our life is used
Product, if toothpaste not only has the function of fresh breath, pole is beneficial to the shield in people oral cavity by the effect of being also equipped with anti-calculus dentalis
Reason.
Chinese patent application CN 105943478A disclose a kind of brilliant white inflammation-diminishing toothpaste, and traditional Chinese medicine ingredients include parts by weight
2~6 parts of 6~10 parts of 2~10 parts of lichen extract, Herba Dendrobii extract, the Bulbus Lilii extract of meter, 3~6 parts of bletilla striata extract, spirit
2~6 parts of 0.5~2 part of sesame extracting solution, 0.5~1 part of fructus lycii extracted solution, 6~8 parts of Rocket ram jet extracting solution and peppermint extracting solution.Wherein
Medicine composition is complicated, content is high, causes production cost high, is unfavorable for promoting.
Chinese patent application CN 107028850A disclose a kind of dendrobium candidum toothpaste with oral restoration,
Including with 0.1~1.0 part of the first dendrobium candidum extract, 1.0~10 parts of bletilla striata extract, 15~35 parts of D-sorbite, water and
8~25 parts of silica, 5~12 parts of glycerine, 1~3 part of borneol, 1~6 part of pearl shell powder, 0.5~3 part of laruyl alcohol sodium sulfovinate, poly- second
1~10 part of glycol, 0.5~3 part of xylitol, 0.3~1 part of sodium cellulose glycolate, 0.1~1 part of Chondrus crispus, xanthans
10~40 parts of 0.1~1 part, 3~8 parts of saccharin sodium, CI191401~3 part, CI420901~3 part and water.The bletilla striata extract
It is refrigerated after sodium chloride solution impregnates by the bletilla striata, reuses the extraction of 10% ethyl alcohol and be made.The toothpaste goes out canker sore, gum
Blood, calculus dentalis removal have preferable effect, but the toothpaste leads to toothpaste using rare dendrobium candidum as main active
It is of high cost, it is unfavorable for promoting.
Bletilla is the dry tuber of the orchid family herbaceos perennial bletilla striata, there is the effect of astringing to arrest bleeding, detumescence and promoting granulation.
It spits blood for hemoptysis, traumatic hemorrhage, sore swollen toxin, chapped skin;Pulmonary tuberculosis hemoptysis, ulcer haemorrhage.Modern medicine study table
Bright, bletilla polysaccharide has antibacterial action, thus is also applied in above-mentioned application CN 107028850A, CN 105943478A white
Splendid achnatherum.At present for the extraction of bletilla polysaccharide mainly using water extraction or ethanol extraction method, but water or ethyl alcohol extraction is applied to obtain
Bletilla polysaccharide application effect it is not notable, particularly when dosage is low substantially without effect, and if improve dosage not only
Production cost is caused to increase, it is difficult to also result in lotion emulsification.
To sum up, it is necessary to the effect of researching and developing a kind of Chinese medicinal toothpaste, bletilla can be given full play to, and can effectively anti-tooth knot
Stone.
Invention content
In order to solve the problems in the existing technology (Chinese medicine preparation of such as toothpaste is complicated, of high cost, anti-calculus dentalis effect
It is bad etc.), inventor is by largely testing, it has been unexpectedly found that adding in sorbierite when adopting and the bletilla striata being extracted with water, obtains
Bletilla striata extract compounded by a certain percentage with pearl shell powder, borneol, and applied in toothpaste, can effectively inhibit plaque, resist
Calculus dentalis effect is apparent.Based on above-mentioned discovery, thereby completing the present invention.
The purpose of the present invention will be further described in detail below reflect and description.
A kind of anti-calculus dentalis Chinese medicinal toothpaste provided by the invention, raw material is prepared including following parts by weight meter:Chinese medicine 5~8
Part, 0.1~0.3 part of saccharin sodium, 0.05~0.1 part of tertiary sodium phosphate, 3~6 parts of glycerine, 40~60 parts of sorbierite, titanium dioxide 0.2~
0.9 part, 0.2~0.6 part of carragheen, 0.5~1 part of carboxymethyl cellulose, 10~15 parts of silicon 201A, 3023~8 parts of silicon, silicon
1033~8 parts, 2~3 parts of lauryl sodium sulfate, 0.1~0.5 part of menthol, 0.01~0.2 part of menthyl lactate, freshener
15~23 parts of WS-230.2~0.9 part, 0.05~0.2 part of methyl hydroxybenzoate, 0.05~0.2 part of ethylparaben and water;It is described
Chinese medicine is by bletilla striata extract, pearl shell powder and borneol according to weight ratio (3~5):1:(1.5~2.5) it forms.
As the preferred embodiment of the present invention, the preparation that the anti-calculus dentalis Chinese medicinal toothpaste includes following parts by weight meter is former
Material:6 parts of Chinese medicine, 0.2 part of saccharin sodium, 0.08 part of tertiary sodium phosphate, 4 parts of glycerine, 50 parts of sorbierite, 0.6 part of titanium dioxide, carragheen
0.4 part, 0.8 part of carboxymethyl cellulose, 13 parts of silicon 201A, 3026 parts of silicon, 1036 parts of silicon, 3 parts of lauryl sodium sulfate, peppermint
0.3 part of brain, 0.1 part of menthyl lactate, WS-230.5 parts of freshener, 0.1 part of methyl hydroxybenzoate, 0.1 part of ethylparaben and water
20 parts;The Chinese medicine is by bletilla striata extract, pearl shell powder and borneol according to weight ratio 4:1:2 compositions.
Further, the bletilla striata extract is made by the following method:The bletilla striata is taken, adds in the bletilla striata 4~6 times of weight of weight
Sorbitol aqueous solution, impregnate 0.5~1h, 2~3h of heating and refluxing extraction, filtering, filter vacuum is concentrated under reduced pressure into original volume
1/5~1/6, bletilla striata extract is made.
Further, in the sorbitol aqueous solution, the weight ratio of sorb alcohol and water is 1:(2~4).
For sorbierite since price is low, performance of keeping humidity is good, thus is widely used in toothpaste as moisturizer, and
Larger proportion is accounted in toothpaste.And the chemical property of sorbierite is stablized relatively, has polyhydroxy structure, and it is soluble easily in water, it is steady to heat
Fixed, therefore, inventor is attempted using sorbierite (i.e. commercially available 70% liquid sorbitol) as the Extraction solvent of the bletilla striata, and utilization is similar
The principle to mix, it would be desirable to a kind of good bletilla polysaccharide mixture of application effect is obtained, if studies have found that with 70%
Liquid sorbitol can not effectively extract the active constituent in the bletilla striata, show as being applied in toothpaste without bright as Extraction solvent
Aobvious antibacterial and the effect of anti-calculus dentalis.Thus inventor has shown that mass percent concentration is 14% by a large number of experiments screening
~23.3% sorbitol aqueous solution (water being added to prepare to obtain using 70% liquid sorbitol), using the sorbitol aqueous solution as
Extraction solvent, obtained bletilla striata extract are applied in toothpaste, have the effect of good antibacterial action and anti-calculus dentalis.Together
When, inventor also found compounds the bletilla striata extract with pearl shell powder, borneol by a certain percentage, and three kinds of component collaborations can press down
Plaque processed, anti-calculus dentalis, but if proportions change, function and effect significantly weaken.In addition, use the sorbierite water
The bletilla striata extract that solution is obtained as Extraction solvent, it is good with the compatibility of lotion of toothpaste, it is easy to emulsify, is brought to toothpaste production
Facility, while toothpaste stable system obtained.Inventor speculates, uses a concentration of 14%~23.3% sorbitol aqueous solution
As Extraction solvent, you can the water soluble ingredient of the bletilla striata is extracted, also the extractable ingredient for being dissolved in sorbierite, and these active constituents
It is cooperateed with pearl shell powder, borneol, the good application effect of acquisition, and due to containing sorbierite in bletilla striata extract system,
And sorbierite is also applied in toothpaste, thus the bletilla striata extract and the compatibility of lotion of toothpaste are good.
Correspondingly, the present invention also provides the preparation method of above-mentioned anti-calculus dentalis Chinese medicinal toothpaste, following steps are specifically included:
S1, the bletilla striata is taken, adds in the sorbitol aqueous solution of the bletilla striata 4~6 times of weight of weight, impregnated 0.5~1h, be heated to reflux carrying
2~3h is taken, is filtered, filter vacuum is concentrated under reduced pressure into the 1/5~1/6 of original volume, and bletilla striata extract is made;
S2, the methyl hydroxybenzoate and ethylparaben for taking formula ratio add in methyl hydroxybenzoate and ethylparaben total weight 4
The water of~6 times of weight stirs to being completely dissolved, obtains antiseptic solution, spare;
S3, the sorbierite of formula ratio and glycerine are mixed in glue pot, add in tertiary sodium phosphate, stirring to being completely dissolved,
Then carragheen, sodium carboxymethylcellulose are added in, wetting stirring adds the water of formula ratio, stirs, and makes manufactured glue in equal
Even translucent viscous shape liquid stores 12h, the glue that must be prepared;
S4, by the saccharin sodium of antiseptic solution, glue and formula ratio, titanium dioxide, silicon 201A, silicon 302, silicon 103, dodecane
Base sodium sulphate, bletilla striata extract, pearl shell powder, borneol, input, which are blocked, closes in pot, stirs 30~45min, is subsequently added into formula ratio
Menthol, menthyl lactate and freshener WS-23 stir 10~15min, obtain lotion;
S5, gained lotion carry out vacuum outgas, vacuum degree be -0.096MPa, the time be 45~65min, lotion after degassing
2 days are stood, is dispensed to get anti-calculus dentalis Chinese medicinal toothpaste.
Further, in the sorbitol aqueous solution, the weight ratio of sorb alcohol and water is 1:(2~4).
Therefore, compared with prior art, advantage of the invention is that:
(1) the anti-calculus dentalis Chinese medicinal toothpaste of the present invention can not only inhibit oral cavity harmful bacteria, and fresh breath goes halitosis, simultaneously
It can effectively inhibit and reduce plaque, slow down the formation of calculus dentalis, there is good anti-calculus dentalis effect, and toothpaste of the present invention
Formula it is simple, active component content is few, and cost of material is low, and stable system, safety can be used for a long time.
(2) preparation method of the anti-calculus dentalis Chinese medicinal toothpaste of the present invention is simple, and condition is controllable, and production cost is low, can scale
Production, can promote and apply.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail.
The raw materials used present invention is conventional commercial commodity.For example, sorbierite of the present invention is active principle content
For 70% liquid sorbitol, purchased from Shandong Tianli Pharmaceutical Co., Ltd.;Silicon 201A, silicon 302 and silicon 103 are purchased from Hunan morning twilight
Chemical Co., Ltd.;Pearl shell powder is purchased from Shanghai lark oral health care product Co., Ltd.
Embodiment 1, the anti-calculus dentalis Chinese medicinal toothpaste of the present invention and its preparation
Formula:Chinese medicine 50kg, saccharin sodium 1kg, tertiary sodium phosphate 0.5kg, glycerine 30kg, 70% liquid sorbitol 400kg, titanium
White powder 2kg, carragheen 2kg, carboxymethyl cellulose 5kg, silicon 201A 100kg, silicon 30230kg, silicon 10330kg, dodecyl sulphur
Sour sodium 20kg, menthol 1kg, menthyl lactate 0.1kg, freshener WS-232kg, methyl hydroxybenzoate 0.5kg, ethylparaben
0.5kg and water 150kg;The Chinese medicine is by bletilla striata extract, pearl shell powder and borneol according to weight ratio 3:1:2.5 composition.
Preparation method:
S1, bletilla striata 10kg is taken, adds in 40kg sorbitol aqueous solutions, impregnate 1h, heating and refluxing extraction 2h, filtered, filtrate is true
Sky is concentrated under reduced pressure into the 1/5 of original volume, and bletilla striata extract is made;
S2, the methyl hydroxybenzoate and ethylparaben for taking formula ratio add in 4kg water, stir to being completely dissolved, obtain preservative
Solution, it is spare;
S3,70% liquid sorbitol and glycerine of formula ratio are mixed in glue pot, adds in tertiary sodium phosphate, stir to complete
Then fully dissolved adds in carragheen, sodium carboxymethylcellulose, wetting stirring adds the water of formula ratio, stirs, and makes manufactured
Glue is in uniform translucent viscous shape liquid, stores 12h, the glue that must be prepared;
S4, by the saccharin sodium of antiseptic solution, glue and formula ratio, titanium dioxide, silicon 201A, silicon 302, silicon 103, dodecane
Base sodium sulphate, bletilla striata extract, pearl shell powder, borneol, input, which are blocked, closes in pot, stirs 30min, is subsequently added into the peppermint of formula ratio
Brain, menthyl lactate and freshener WS-23 stir 10min, obtain lotion;
S5, gained lotion carry out vacuum outgas, and vacuum degree is -0.096MPa, time 45min, and lotion stands 2 after degassing
My god, it dispenses to get anti-calculus dentalis Chinese medicinal toothpaste.
In the sorbitol aqueous solution, the weight ratio of sorb alcohol and water is 1:2, i.e., into the liquid sorbitol of 10kg70%
20kg water is added in, the sorbitol aqueous solution that mass percent concentration is 23.3% is made.
Embodiment 2, the anti-calculus dentalis Chinese medicinal toothpaste of the present invention and its preparation
Formula:Chinese medicine 80kg, saccharin sodium 3kg, tertiary sodium phosphate 1kg, glycerine 60kg, 70% liquid sorbitol 600kg, titanium white
Powder 9kg, carragheen 6kg, carboxymethyl cellulose 10kg, silicon 201A 150kg, silicon 30280kg, silicon 10380kg, dodecyl sulphur
Sour sodium 30kg, menthol 5kg, menthyl lactate 2kg, freshener WS-239kg, methyl hydroxybenzoate 2kg, ethylparaben 2kg and
Water 230kg;The Chinese medicine is by bletilla striata extract, pearl shell powder and borneol according to weight ratio 5:1:1.5 composition.
Preparation method:
S1, bletilla striata 10kg is taken, adds in 60kg sorbitol aqueous solutions, impregnate 1h, heating and refluxing extraction 3h, filtered, filtrate is true
Sky is concentrated under reduced pressure into the 1/6 of original volume, and bletilla striata extract is made;
S2, the methyl hydroxybenzoate and ethylparaben for taking formula ratio add in 24kg water, stir to being completely dissolved, obtain anti-corrosion
Agent solution, it is spare;
S3,70% liquid sorbitol and glycerine of formula ratio are mixed in glue pot, adds in tertiary sodium phosphate, stir to complete
Then fully dissolved adds in carragheen, sodium carboxymethylcellulose, wetting stirring adds the water of formula ratio, stirs, and makes manufactured
Glue is in uniform translucent viscous shape liquid, stores 12h, the glue that must be prepared;
S4, by the saccharin sodium of antiseptic solution, glue and formula ratio, titanium dioxide, silicon 201A, silicon 302, silicon 103, dodecane
Base sodium sulphate, bletilla striata extract, pearl shell powder, borneol, input, which are blocked, closes in pot, stirs 45min, is subsequently added into the peppermint of formula ratio
Brain, menthyl lactate and freshener WS-23 stir 15min, obtain lotion;
S5, gained lotion carry out vacuum outgas, and vacuum degree is -0.096MPa, time 65min, and lotion stands 2 after degassing
My god, it dispenses to get anti-calculus dentalis Chinese medicinal toothpaste.
In the sorbitol aqueous solution, the weight ratio of sorb alcohol and water is 1:4, i.e., into the liquid sorbitol of 10kg70%
40kg water is added in, the sorbitol aqueous solution that mass percent concentration is 14% is made.
Embodiment 3, the anti-calculus dentalis Chinese medicinal toothpaste of the present invention and its preparation
Formula:Chinese medicine 60kg, saccharin sodium 2kg, tertiary sodium phosphate 0.8kg, glycerine 40kg, 70% liquid sorbitol 500kg, titanium
White powder 6kg, carragheen 4kg, carboxymethyl cellulose 8kg, silicon 201A 130kg, silicon 30260kg, silicon 10360kg, dodecyl sulphur
Sour sodium 30kg, menthol 3kg, menthyl lactate 1kg, freshener WS-235kg, methyl hydroxybenzoate 1kg, ethylparaben 1kg and
Water 200kg;The Chinese medicine is by bletilla striata extract, pearl shell powder and borneol according to weight ratio 4:1:2 compositions.
Preparation method:
S1, bletilla striata 10kg is taken, adds in 50kg sorbitol aqueous solutions, impregnate 1h, heating and refluxing extraction 3h, filtered, filtrate is true
Sky is concentrated under reduced pressure into the 1/5 of original volume, and bletilla striata extract is made;
S2, the methyl hydroxybenzoate and ethylparaben for taking formula ratio add in 10kg water, stir to being completely dissolved, obtain anti-corrosion
Agent solution, it is spare;
S3,70% liquid sorbitol and glycerine of formula ratio are mixed in glue pot, adds in tertiary sodium phosphate, stir to complete
Then fully dissolved adds in carragheen, sodium carboxymethylcellulose, wetting stirring adds the water of formula ratio, stirs, and makes manufactured
Glue is in uniform translucent viscous shape liquid, stores 12h, the glue that must be prepared;
S4, by the saccharin sodium of antiseptic solution, glue and formula ratio, titanium dioxide, silicon 201A, silicon 302, silicon 103, dodecane
Base sodium sulphate, bletilla striata extract, pearl shell powder, borneol, input, which are blocked, closes in pot, stirs 40min, is subsequently added into the peppermint of formula ratio
Brain, menthyl lactate and freshener WS-23 stir 15min, obtain lotion;
S5, gained lotion carry out vacuum outgas, and vacuum degree is -0.096MPa, time 55min, and lotion stands 2 after degassing
My god, it dispenses to get anti-calculus dentalis Chinese medicinal toothpaste.
In the sorbitol aqueous solution, the weight ratio of sorb alcohol and water is 1:3, i.e., into the liquid sorbitol of 10kg70%
30kg water is added in, the sorbitol aqueous solution that mass percent concentration is 17.5% is made.
Comparative example one
Compared with Example 3, this comparative example differs only in:Using water as Extraction solvent, i.e. step S1, take the bletilla striata
10kg adds in 50kg water, impregnates 1h, heating and refluxing extraction 3h, filtering, and filter vacuum is concentrated under reduced pressure into the 1/5 of original volume, is made
Bletilla striata extract.
Comparative example two
Compared with Example 3, this comparative example differs only in:Liquid sorbitol using commercially available 70% is molten as extracting
Agent.
Comparative example three
Compared with Example 3, this comparative example differs only in:The Chinese medicine is by bletilla striata extract, pearl shell powder and ice
Piece is according to weight ratio 4:2:1 composition.
Comparative example four
With reference to the embodiment 7 of CN 107028850A, toothpaste is made.
Comparative example five
With reference to the embodiment 7 of CN 107028850A, but the first dendrobium candidum extract is not added, toothpaste is made.
Test example one, the examination of the stability of Chinese medicinal toothpaste of the present invention
1st, content of the test:
(1) Examples 1 to 3 toothpaste sample is put into 50 DEG C of baking ovens and stored, taken out after 6 months, split toothpaste, observe tooth
The situation of change of cream.
(2) Examples 1 to 3 toothpaste sample is tried to store in normal temperature condition undercarriage, is taken out after 24 months, split toothpaste, examine
Look into the situation of change of toothpaste.
2nd, result of the test:
Examples 1 to 3 toothpaste is stored 6 months under the conditions of 50 DEG C and is stored 24 months under normal temperature condition, splits lotion
Normally, there are not the abnormal conditions such as shrinking away from theshell, lotion spilling nozzle, separation water outlet, still keep fine and smooth uniform shape, and fragrance color and luster
Normally.Illustrate that the stability of Chinese medicinal toothpaste of the present invention is good, and bletilla striata extract of the present invention is prompted easily to emulsify, with lotion
Compatibility is good.
Test example two, Chinese medicinal toothpaste of the present invention examine or check the function and effect of oral cavity common bacteria
1st, material:
(1) bacterial species:The bacterium of use is international standard strain, including streptococcus mutans (Streptococcus
Mutans, ATCC25175), Streptococcus sanguis (Streptococcus sanguis, ATCC 10556), actinomyces viscosus
(Actinomyces viscosus, ATCC19246) and Candida albicans (Candida albicans, ATCC 76615).
(2) bacteria culture media:For Tryptose soy broth bouillon.Preparation method is Tryptose soy meat soup 30g, basic
Agar 15g, sterilize the raw water 1L that reduces phlegm and internal heat.
(3) inoculum:For 3% Tryptose soy meat soup 200mL.Preparation method adds for Tryptose soy meat soup 6g goes out
Bacterium is reduced phlegm and internal heat raw water 200mL.
(4) filter paper:Millipak-40, Milipore roundlet filter paper.
2nd, method:
Utilize the antibiotic property of diffusion method assessment toothpaste.Blank control group:The raw water of reducing phlegm and internal heat of sterilizing.It is Example 1~3, right
Each 50mg of one~five toothpaste of ratio, with pyrogen removal water 1:1 dilution.
Inoculum uniform crossover is applied on the culture medium of culture dish, culture dish is placed in 37 DEG C of constant temperature incubator
In for 24 hours, cultivate each 13 of the culture dish of each bacterium.Respectively the 1 of each experiment toothpaste:1 dilution and the raw water of reducing phlegm and internal heat of sterilizing
With 10 μ l capillary burettes equivalent drop on roundlet filter paper, then the 3 roundlet filter papers that toothpaste of the same race or raw water of reducing phlegm and internal heat will be stained with
The middle section symmetrically being attached on culture medium is detected the concentration of each toothpaste in each bacteria culture media.
Finally culture dish is placed in 37 DEG C of constant temperature incubator and cultivated for 24 hours, 3 similar round antibacterial areas after measuring for 24 hours in culture dish
The diameter in domain is simultaneously averaged.Carry out the antibiotic property of the analysis and assessment toothpaste with the size of antibacterial region diameter.If the toothpaste has
There is antibiotic property, then antibacterial region can be shown on culture medium, diameter is bigger to represent that antibiotic property is stronger.
3rd, result:
Comparison of the 1 each toothpaste of table to 4 kinds of oral cavity common bacteria antibacterial region diameters
From upper table 1:
(1) blank control group has no generation antibacterial region, and 1~3 Chinese medicinal toothpaste of the embodiment of the present invention to streptococcus mutans,
This 4 kinds of oral cavity common bacterias of Streptococcus sanguis, actinomyces viscosus and Candida albicans generate apparent antibacterial region, illustrate in the present invention
Medicine toothpaste has apparent antibacterial action to streptococcus mutans, Streptococcus sanguis, actinomyces viscosus and Candida albicans, wherein, with reality
The antibacterial action for applying 3 Chinese medicinal toothpaste of example is most apparent.Streptococcus mutans, Streptococcus sanguis, actinomyces viscosus and Candida albicans are oral cavities
Common bacteria, they can cause the common disease in oral cavity, such as dental caries, periodontosis and oral mucosal disease.Wherein, streptococcus mutans are
Plaque Early Earth bacterium, toothpaste of the present invention have significant inhibiting effect to streptococcus mutans, prompt toothpaste of the present invention that can press down
Plaque processed, so as to have the effect of anti-calculus dentalis.
(2) Extraction solvent of the comparative example one using water as the bletilla striata, the bletilla striata extract as a result obtained are applied in toothpaste, phase
Than in Examples 1 to 3, antibacterial action is very weak;Extraction solvent of the comparative example two using 70% liquid sorbitol as the bletilla striata, as a result
To bletilla striata extract be applied to toothpaste in, do not have antibacterial action substantially.Comparative example three changes bletilla striata extract, pearl shell
The proportioning of powder and borneol, compared to Examples 1 to 3, antibacterial action is decreased obviously.
(3) comparative example four is the toothpaste of prior art CN 107028850A, slightly poor to the inhibiting effect of Candida albicans
In the present invention;Comparative example five is existing CN 107028850A but the toothpaste without the first dendrobium candidum extract, compared to implementation
Example 1~3 and comparative example four, antibacterial action is decreased obviously.
The in vitro test of test example three, the anti-calculus dentalis of Chinese medicinal toothpaste of the present invention
1st, toothpaste is tested:One~five toothpaste of Examples 1 to 3 and comparative example, blank control toothpaste:Reality without traditional Chinese medicine ingredients
Apply 3 toothpaste of example.
2nd, test method:
Plaque is grown and mineralization model is that plaque is cultivated from people's saliva, its mineralising is then made in mineralized liquid, and
And mineralising bacterial plaque is handled with the dentifrice slurry containing different activities ingredient, 1 time a day, each 30s, continue 10d, finally according to
It is secondary to be parsed bacterial plaque with sodium hydroxide and hydrogen chloride, analyze mixed liquor in calcium ion content, thus judge different activities into
Divide the effect of anti-calculus dentalis.If calcium ion content is less in solution, the calculus dentalis amount formed is less, illustrates that the group is used
Toothpaste have stronger anti-calculus dentalis effect.4th, result of the test:
The content of calcium ion and different toothpaste are to the removal rate of calculus dentalis in 2 plaque of table
Test toothpaste | Average calcium content (μ g) in plaque | Anti- calculus dentalis efficiency * (%) |
Blank control | 1229.4 | 0 |
Embodiment 1 | 367.6 | 70.1 |
Embodiment 2 | 378.6 | 69.2 |
Embodiment 3 | 327.0 | 73.4 |
Comparative example one | 1033.9 | 15.9 |
Comparative example two | 1213.5 | 1.3 |
Comparative example three | 730.3 | 40.6 |
Comparative example four | 319.6 | 74.0 |
Comparative example five | 998.3 | 18.8 |
From upper table 2:
The comparison of mineralization model is grown by microorganism, 1~3 Chinese medicinal toothpaste of the embodiment of the present invention is to the removal rate of calculus dentalis
Respectively 70.1%, 69.2% and 73.4%, have stronger anti-calculus dentalis effect, and four existing toothpaste of comparative example also have compared with
Strong anti-calculus dentalis effect, effect are close with Chinese medicinal toothpaste of the present invention.Comparative example two is right substantially without the effect of anti-calculus dentalis
Ratio one, comparative example five have weaker anti-calculus dentalis effect, comparative example three then in medium anti-calculus dentalis effect.This experiment generates
Data result it is similar with the result of test example two.
The clinical test of test example four, the anti-calculus dentalis of Chinese medicinal toothpaste of the present invention
1st, subjects:Meet and be included in and the easy adult male and women for forming calculus dentalis of exclusion criteria.
2nd, operating process:
1) it needs to clean the teeth to subject after baseline inspection, removes dental calculus, bacterial plaque, soft dirt are removed with rubber polishing cup,
Carry out oral hygiene instyuctions, it is desirable that all subjects uniformly using bass brushings, then start granting and use product.
2) this experiment 6 months by a definite date carry out clinical examination three times (baseline, 3 months and 6 months), and experiment is completed, statistics knot
It is taken off after beam blind.
3) for ease of understanding and strengthen the compliance of subject, monthly follow-up is taken to supplement toothpaste, with supervise subject and
Adverse reaction etc. is understood in time.
3rd, experiment grouping and operation instruction:
1) experiment grouping:Test 1 group:The Chinese medicinal toothpaste of embodiment 1 tests 2 groups:The Chinese medicinal toothpaste of embodiment 2 tests 3 groups:
The Chinese medicinal toothpaste control group of embodiment 3:Plant sodium toothpaste (is purchased from Tongxiang Xinyang Food Additives Co., Ltd.)
2) granting of product:Each group provides the tooth paste product of unitizing and same producer, the toothbrush of same model.
3) requirement:Tested period can only use the toothpaste and toothbrush provided, must not use other toothpaste, toothbrush or mouth
Chamber amenities, such as mouthwash, dental floss.Daily morning and evening respectively using 1 time, each dosage must be covered with entire toothbrush bristle (about
2g), usage time about 3 minutes.
4th, test method:
1) number of subjects:It tests 1 group, 2 groups of experiment, test 3 groups and each 80 people of control group
2) using the clinical testing procedure of random, double blind, control.
5th, observation item and Index for examination:
1) it using V-M indexs, is designed by Volpe&Manhold (1965), for observing the situation of evaluation calculus dentalis, mainly
Assess the amount of calculus dentalis.
2) inspection method:Using the standard periodontal probe indexed by millimeter, after tooth lingual surface is dried, before checking under 6
The lingual surface of tooth.Probe is placed on the center line of tooth lingual surface, parallel with long axis of tooth, measures the maximum height of calculus dentalis on gum;Probe leads to
The mesio-incisal angle of tooth is crossed, measures the maximum height of lingual surface distal margin calculus dentalis;It is near to measure lingual surface by the disto-incisal angle of tooth for probe
The maximum height of middle edge calculus dentalis.Each tooth lingual surface measures three times, is measured every time as calculus dentalis is denoted as in scale 3 or more than 3
3。
3) score standard:The minimum score measured every time is 0, is secondly 0.5,1,2,3, and the maximum score of each tooth is 9,
Everyone maximum score is 54, and the maximum score detected every time is 3.
4) it has no adverse reaction after use.
5) examiner:Toothpaste has been checked using forward and backward clinical indexes by a doctor.
6th, result of the test:
3 two groups of subjects of table use the comparison of V-M indexes before and after toothpaste
From upper table 3:
The V-M index mean no difference of science of statistics (P of four groups of subjects when checking for the first time>0.05);Through clean after baseline inspection
Tooth and oral hygiene instyuctions, during using toothpaste 3 months, the formation no statistical difference difference (P of four groups of subject's calculus dentalis>
0.05), when using toothpaste 6 months, compared with the control group, 1 group of experiment, 2 groups of experiment and the shape for testing 3 groups of subject's calculus dentalis
Into there is significant difference (P<0.05).
Four groups of subjects after toothpaste using not occurring adverse reaction.
7th, conclusion:
This experimental study shows in 6 months by a definite date random, double blind, check experiment:
(1) compared to control group toothpaste, calculus dentalis can preferably be slowed down using 3 groups of 1 group of experiment, 2 groups of experiment and experiment
It is formed, i.e., 1~3 Chinese medicinal toothpaste of the embodiment of the present invention has the effect of good anti-calculus dentalis.
(2) 1 group is tested, 2 groups is tested and tests 3 groups of subjects using having no adverse reaction after toothpaste, is i.e. the embodiment of the present invention 1
~3 Chinese medicinal toothpastes safety, can be used for a long time.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, several simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (6)
1. a kind of anti-calculus dentalis Chinese medicinal toothpaste, which is characterized in that prepare raw material including following parts by weight meter:5~8 parts of Chinese medicine,
0.1~0.3 part of saccharin sodium, 0.05~0.1 part of tertiary sodium phosphate, 3~6 parts of glycerine, 40~60 parts of sorbierite, titanium dioxide 0.2~0.9
Part, 0.2~0.6 part of carragheen, 0.5~1 part of carboxymethyl cellulose, 10~15 parts of silicon 201A, 3023~8 parts of silicon, silicon 1033~
8 parts, 2~3 parts of lauryl sodium sulfate, 0.1~0.5 part of menthol, 0.01~0.2 part of menthyl lactate, freshener WS-
15~23 parts of 230.2~0.9 parts, 0.05~0.2 part of methyl hydroxybenzoate, 0.05~0.2 part of ethylparaben and water;The Chinese medicine
By bletilla striata extract, pearl shell powder and borneol according to weight ratio (3~5):1:(1.5~2.5) it forms.
2. anti-calculus dentalis Chinese medicinal toothpaste as described in claim 1, which is characterized in that prepare raw material including following parts by weight meter:
6 parts of Chinese medicine, 0.2 part of saccharin sodium, 0.08 part of tertiary sodium phosphate, 4 parts of glycerine, 50 parts of sorbierite, 0.6 part of titanium dioxide, carragheen 0.4
Part, 0.8 part of carboxymethyl cellulose, 13 parts of silicon 201A, 3026 parts of silicon, 1036 parts of silicon, 3 parts of lauryl sodium sulfate, menthol
0.3 part, 0.1 part of menthyl lactate, WS-230.5 parts of freshener, 0.1 part of methyl hydroxybenzoate, 0.1 part of ethylparaben and water 20
Part;The Chinese medicine is by bletilla striata extract, pearl shell powder and borneol according to weight ratio 4:1:2 compositions.
3. anti-calculus dentalis Chinese medicinal toothpaste as claimed in claim 1 or 2, which is characterized in that the bletilla striata extract passes through with lower section
Method is made:The bletilla striata is taken, adds in the sorbitol aqueous solution of the bletilla striata 4~6 times of weight of weight, impregnates 0.5~1h, heating and refluxing extraction 2
~3h, filtering, filter vacuum are concentrated under reduced pressure into the 1/5~1/6 of original volume, and bletilla striata extract is made.
4. anti-calculus dentalis Chinese medicinal toothpaste as claimed in claim 3, which is characterized in that in the sorbitol aqueous solution, sorbierite and
The weight ratio of water is 1:(2~4).
5. the preparation method of anti-calculus dentalis Chinese medicinal toothpaste as described in claim 1, which is characterized in that include the following steps:
S1, the bletilla striata is taken, adds in the sorbitol aqueous solution of the bletilla striata 4~6 times of weight of weight, impregnate 0.5~1h, heating and refluxing extraction 2
~3h, filtering, filter vacuum are concentrated under reduced pressure into the 1/5~1/6 of original volume, and bletilla striata extract is made;
S2, the methyl hydroxybenzoate and ethylparaben for taking formula ratio add in methyl hydroxybenzoate and ethylparaben total weight 4~6
The water of times weight stirs to being completely dissolved, obtains antiseptic solution, spare;
S3, the sorbierite of formula ratio and glycerine are mixed in glue pot, adds in tertiary sodium phosphate, stirred to being completely dissolved, then
Carragheen, sodium carboxymethylcellulose are added in, wetting stirring adds the water of formula ratio, stirs, and makes manufactured glue in uniformly half
Transparent viscous shape liquid stores 12h, the glue that must be prepared;
S4, by the saccharin sodium of antiseptic solution, glue and formula ratio, titanium dioxide, silicon 201A, silicon 302, silicon 103, dodecyl sulphur
Sour sodium, bletilla striata extract, pearl shell powder, borneol, input, which are blocked, closes in pot, stirs 30~45min, is subsequently added into the peppermint of formula ratio
Brain, menthyl lactate and freshener WS-23 stir 10~15min, obtain lotion;
S5, gained lotion carry out vacuum outgas, and vacuum degree is -0.096MPa, and the time is 45~65min, and lotion stands 2 after degassing
My god, it dispenses to get anti-calculus dentalis Chinese medicinal toothpaste.
6. the preparation method of anti-calculus dentalis Chinese medicinal toothpaste as claimed in claim 5, which is characterized in that the sorbitol aqueous solution
In, the weight ratio of sorb alcohol and water is 1:(2~4).
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CN109998975A (en) * | 2019-05-24 | 2019-07-12 | 福建中合医药股份有限公司 | A kind of efficient toothpaste |
CN110179742A (en) * | 2019-07-09 | 2019-08-30 | 浙江爱尚日用品有限公司 | A kind of health Chinese medicinal toothpaste of tooth-whitening |
CN110652461A (en) * | 2019-10-28 | 2020-01-07 | 严巧文 | Health-care whitening toothpaste |
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US20220160597A1 (en) * | 2020-11-20 | 2022-05-26 | Howard Frysh | Dental calculus removal |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106221912A (en) * | 2016-08-22 | 2016-12-14 | 广西中烟工业有限责任公司 | A kind of process for purification containing Herba Menthae Rotundifoliae perfume material and application |
CN107028850A (en) * | 2017-04-24 | 2017-08-11 | 上海玉慈生物科技有限公司 | Dendrobium candidum toothpaste and its preparation technology with oral restoration function |
-
2018
- 2018-01-24 CN CN201810075182.7A patent/CN108175737B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106221912A (en) * | 2016-08-22 | 2016-12-14 | 广西中烟工业有限责任公司 | A kind of process for purification containing Herba Menthae Rotundifoliae perfume material and application |
CN107028850A (en) * | 2017-04-24 | 2017-08-11 | 上海玉慈生物科技有限公司 | Dendrobium candidum toothpaste and its preparation technology with oral restoration function |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109998975A (en) * | 2019-05-24 | 2019-07-12 | 福建中合医药股份有限公司 | A kind of efficient toothpaste |
CN110179742A (en) * | 2019-07-09 | 2019-08-30 | 浙江爱尚日用品有限公司 | A kind of health Chinese medicinal toothpaste of tooth-whitening |
CN110652461A (en) * | 2019-10-28 | 2020-01-07 | 严巧文 | Health-care whitening toothpaste |
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