CN108175737B - 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 PDF

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CN108175737B
CN108175737B CN201810075182.7A CN201810075182A CN108175737B CN 108175737 B CN108175737 B CN 108175737B CN 201810075182 A CN201810075182 A CN 201810075182A CN 108175737 B CN108175737 B CN 108175737B
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toothpaste
silicon
bletilla striata
calculus dentalis
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CN108175737A (en
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林创有
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Sanjiao Dailychemical Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
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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 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 glycerol, 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, 0.2~0.9 part of freshener WS-23, 0.05~0.2 part of methylparaben, 0.05~0.2 part and 15~23 parts of water of ethylparaben.Toothpaste of the present invention can effectively inhibit plaque, slow down the formation of calculus dentalis, have the effect of anti-calculus dentalis.

Description

A kind of anti-calculus dentalis Chinese medicinal toothpaste and preparation method thereof
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 technique
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, cell-free dental cuticle, and main component is substantially similar to saliva, contains mucoprotein, sugar Albumen, blood-group antigen and immunoglobulin, some of them ingredient can promote bacterium to stick refined surface, play the function of receptor Energy.Then, intraoral bacterium is attached on film successively by substances such as protein, polysaccharide, the lipoteichoicacids on its surface, Bacterium forms complicated flora, using 10~30 days, bacterial plaque mature reached by sticking and copolymerization is interconnected, is proliferated To peak.On bacterial plaque surface, because the cell that mineral mineralization, swill and the necrosis in saliva fall off participates in, in bacterial plaque shape At 2~14 days can calcification, be hardened and form calculus.
Periodontal disease is that the mankind are distributed most wide one of 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, and to safeguard periodontal health, it is fixed to advocate people 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 can easily damage enamel by the way of mechanical removal for a long time.Thus use 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 Pole the effect of being also equipped with anti-calculus dentalis, is beneficial to the shield in people oral cavity if toothpaste not only has the function of fresh breath by product Reason.
Chinese patent application CN 105943478A discloses 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 0.5~2 part of sesame extracting solution, 0.5~1 part of fructus lycii extracted solution, 6~8 parts of pyracantha fortuneana fruit extracting solution and 2~6 parts of peppermint extracting solution.Wherein Medicine composition is complicated, content is high, leads to high production cost, is unfavorable for promoting.
Chinese patent application CN 107028850A discloses a kind of dendrobium candidum toothpaste with oral restoration function, 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 glycerol, 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, xanthan gum 0.1~1 part, 3~8 parts of saccharin sodium, CI191401~3 part, CI420901~3 part and 10~40 parts of 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 at 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 also applies in above-mentioned application CN 107028850A, CN 105943478A white Splendid achnatherum.Water extraction or ethanol extraction method are mainly used for the extraction of bletilla polysaccharide at present, but applies water or ethyl alcohol to extract and obtains Bletilla polysaccharide application effect it is not significant, especially when dosage is low substantially without effect, and if improve dosage not only Cause production cost 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.
Summary of the invention
In order to solve the problems in the existing technology (Chinese medicine preparation complexity, at high cost, the anti-calculus dentalis effect of such as toothpaste It is bad etc.), inventor is by largely testing, it has been unexpectedly found that sorbierite is added 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 be applied to toothpaste in, can effectively inhibit plaque, resist Calculus dentalis effect is obvious.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, prepares raw material 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 glycerol, 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-230.2~0.9 part, 0.05~0.2 part of methylparaben, 0.05~0.2 part of ethylparaben and 15~23 parts of 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 a preferred embodiment of the present invention, the anti-calculus dentalis Chinese medicinal toothpaste includes that the preparation of 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 glycerol, 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 methylparaben, 0.1 part of ethylparaben and water 20 parts;The Chinese medicine is made of bletilla striata extract, pearl shell powder and borneol according to weight ratio 4:1:2.
Further, the bletilla striata extract is made by the following method: taking the bletilla striata, 4~6 times of weight of bletilla striata weight are added 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 Biggish specific gravity is accounted in toothpaste.And the chemical property of sorbierite is relatively stable, has polyhydroxy structure, and it is soluble easily in water, it is steady to heat Fixed, therefore, inventor attempts 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, studies have found that if with 70% Liquid sorbitol can not effectively extract the active constituent in the bletilla striata as Extraction solvent, show as being applied in toothpaste without bright The effect of aobvious antibacterial and 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 (adding water to prepare to obtain using 70% liquid sorbitol), use 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 obviously weaken.In addition, using 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 Convenience, while toothpaste stable system obtained.Inventor's supposition, the sorbitol aqueous solution for the use of concentration being 14%~23.3% As Extraction solvent, that is, it can extract the water soluble ingredient of the bletilla striata, 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 methods of above-mentioned anti-calculus dentalis Chinese medicinal toothpaste, specifically includes the following steps:
S1, the bletilla striata is taken, the sorbitol aqueous solution of 4~6 times of weight of bletilla striata weight is added, impregnated 0.5~1h, be heated to reflux and mention 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;
Methylparaben and ethylparaben total weight 4 is added in S2, the methylparaben and ethylparaben for taking formula ratio The water of~6 times of weight stirs to being completely dissolved, obtains antiseptic solution, spare;
S3, the sorbierite of formula ratio and glycerol mixed in glue pot, is added tertiary sodium phosphate, stirring to being completely dissolved, Then carragheen, sodium carboxymethylcellulose is added, 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, investment, 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, and vacuum degree is -0.096MPa, and the time is 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, present invention has an advantage 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 be effectively suppressed 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, it is 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, glycerol 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, methylparaben 0.5kg, ethylparaben 0.5kg and water 150kg;The Chinese medicine is made of bletilla striata extract, pearl shell powder and borneol according to weight ratio 3:1:2.5.
Preparation method:
S1, bletilla striata 10kg is taken, 40kg sorbitol aqueous solution is added, 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;
4kg water is added in S2, the methylparaben and ethylparaben for taking formula ratio, stirs to being completely dissolved, obtains preservative Solution, it is spare;
S3,70% liquid sorbitol and glycerol of formula ratio mixed in glue pot, is added tertiary sodium phosphate, stirring is to complete Then carragheen, sodium carboxymethylcellulose is added in fully dissolved, 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, investment, 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 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, 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, glycerol 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, methylparaben 2kg, ethylparaben 2kg and Water 230kg;The Chinese medicine is made of bletilla striata extract, pearl shell powder and borneol according to weight ratio 5:1:1.5.
Preparation method:
S1, bletilla striata 10kg is taken, 60kg sorbitol aqueous solution is added, 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;
24kg water is added in S2, the methylparaben and ethylparaben for taking formula ratio, stirs to being completely dissolved, obtains anti-corrosion Agent solution, it is spare;
S3,70% liquid sorbitol and glycerol of formula ratio mixed in glue pot, is added tertiary sodium phosphate, stirring is to complete Then carragheen, sodium carboxymethylcellulose is added in fully dissolved, 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, investment, 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 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, 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, glycerol 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, methylparaben 1kg, ethylparaben 1kg and Water 200kg;The Chinese medicine is made of bletilla striata extract, pearl shell powder and borneol according to weight ratio 4:1:2.
Preparation method:
S1, bletilla striata 10kg is taken, 50kg sorbitol aqueous solution is added, 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;
10kg water is added in S2, the methylparaben and ethylparaben for taking formula ratio, stirs to being completely dissolved, obtains anti-corrosion Agent solution, it is spare;
S3,70% liquid sorbitol and glycerol of formula ratio mixed in glue pot, is added tertiary sodium phosphate, stirring is to complete Then carragheen, sodium carboxymethylcellulose is added in fully dissolved, 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, investment, 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 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, the sorbitol aqueous solution that mass percent concentration is 17.5% is made.
Comparative example one
Compared with Example 3, the difference of this comparative example is only that: being used water as Extraction solvent, is i.e. step S1, is taken the bletilla striata 50kg water is added in 10kg, 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, the difference of this comparative example is only that: using commercially available 70% liquid sorbitol molten as extracting Agent.
Comparative example three
Compared with Example 3, the difference of this comparative example is only that: the Chinese medicine is by bletilla striata extract, pearl shell powder and ice Piece is formed according to weight ratio 4:2:1.
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
1, content of the test:
(1) Examples 1 to 3 toothpaste sample is put into 50 DEG C of baking ovens and is stored, taken out after 6 months, split toothpaste, observe tooth The situation of change of cream.
(2) it by the frame examination storage under normal temperature conditions of Examples 1 to 3 toothpaste sample, is taken out after 24 months, splits toothpaste, examine Look into the situation of change of toothpaste.
2, test result:
Examples 1 to 3 toothpaste is stored 6 months under the conditions of 50 DEG C and is stored 24 months under normal temperature conditions, and lotion is splitted 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 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 to be easy emulsification, 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
1, 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, basis 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.
2, 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 is diluted with pyrogen removal water 1:1.
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, culture each 13, culture dish of every kind of bacterium.Respectively the 1:1 dilution of each test toothpaste and the raw water of reducing phlegm and internal heat of sterilizing With 10 μ l capillary burette 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 in concentration of the every kind of bacteria culture media to every kind of toothpaste. Finally culture dish is placed in 37 DEG C of constant temperature incubator and is cultivated for 24 hours, 3 similar round antibacterial areas after measurement 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 can show antibacterial region on culture medium, diameter is bigger, and expression antibiotic property is stronger.
3, result:
Comparison of each toothpaste of table 1 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 obvious.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, 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 proportion 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 is free of the toothpaste of 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
1, toothpaste: one~five toothpaste of Examples 1 to 3 and comparative example, blank control toothpaste: the reality without traditional Chinese medicine ingredients is tested Apply 3 toothpaste of example.
2, test method:
Plaque growth and mineralization model are 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 determine different activities at 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.4, test result:
The removal rate of the content of calcium ion and different toothpaste to calculus dentalis in 2 plaque of table
Test toothpaste In plaque average calcium content (μ g) 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, removal rate of 1~3 Chinese medicinal toothpaste of the embodiment of the present invention to calculus dentalis are grown by microorganism Respectively 70.1%, 69.2% and 73.4%, have stronger anti-calculus dentalis effect, and the existing toothpaste of comparative example four also have compared with Strong anti-calculus dentalis effect, effect are close with Chinese medicinal toothpaste of the present invention.Effect of the comparative example two substantially without anti-calculus dentalis, it is right Ratio one, comparative example five have weaker anti-calculus dentalis effect, comparative example three then in medium anti-calculus dentalis effect.This test 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
1, subjects: meet and be included in and the adult male and women of the calculus dentalis easy to form of exclusion criteria.
2, operating process:
1) it needs to clean the teeth to subject after baseline inspection, removes dental calculus, remove bacterial plaque, soft dirt with rubber polishing cup, Carry out oral hygiene instyuctions, it is desirable that all subjects uniformly use bass brushing, then start granting and use product.
2) this test 6 months by a definite date carry out clinical examination (baseline, 3 months and 6 months) three times, and test is completed, statistics is tied It is taken off after beam blind.
3) to take monthly follow-up to supplement toothpaste convenient for the compliance that understands and reinforce subject, with supervise subject and Adverse reaction etc. is understood in time.
3, test grouping and operation instruction:
1) test grouping: 1 group of test: 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 the toothbrush of same producer, 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.It respectively uses 1 time daily morning and evening, each dosage must be covered with entire toothbrush bristle (about 2g), using the time about 3 minutes.
4, test method:
1) number of subjects: 1 group of test, 2 groups of test, test 3 groups and each 80 people of control group
2) using random, double blind, control clinical testing procedure.
5, observation item and Index for examination:
1) V-M index is used, is designed by Volpe&Manhold (1965), for observing the case where evaluating calculus dentalis, mainly Assess the amount of calculus dentalis.
2) inspection method: using the standard periodontal probe by millimeter indexing, after the drying of tooth lingual surface, before checking under 6 The lingual surface of tooth.Probe is placed on the middle line of tooth lingual surface, parallel with long axis of tooth, measures the maximum height of calculus dentalis on gum;Probe is logical The mesio-incisal angle of tooth is crossed, the maximum height of lingual surface distal margin calculus dentalis is measured;It is close 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, and measurement such as calculus dentalis is denoted as in scale 3 or more than 3 every time 3。
3) scoring criteria: 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.
6, test result:
3 two groups of subjects of table use the comparison of V-M index before and after toothpaste
From upper table 3:
The V-M index mean no difference of science of statistics (P > 0.05) of four groups of subjects when checking for the first time;Through clean after baseline inspection Tooth and oral hygiene instyuctions, when using toothpaste 3 months, the formation no statistical difference difference of four groups of subject's calculus dentalis (P > 0.05), when using toothpaste 6 months, compared with the control group, 1 group of test, 2 groups of test and the shape for testing 3 groups of subject's calculus dentalis At there is statistical difference (P < 0.05).
Four groups of subjects are not using occurring adverse reaction after toothpaste.
7, 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 test, 2 groups of test and test 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) it tests 1 group, test 2 groups and tests 3 groups of subjects using having no adverse reaction after toothpaste, 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, and it cannot be said that Specific implementation of the invention is only limited to these instructions.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, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention Protection scope.

Claims (2)

1. a kind of anti-calculus dentalis Chinese medicinal toothpaste, which is characterized in that be prepared by the raw material of 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 glycerol, 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, 302 3~8 parts of silicon, silicon 103 3~8 parts, 2~3 parts of lauryl sodium sulfate, 0.1~0.5 part of menthol, 0.01~0.2 part of menthyl lactate, freshener 0.2~0.9 part of WS-23,0.05~0.2 part of methylparaben, 0.05~0.2 part of ethylparaben and 15~23 parts of 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;
The bletilla striata extract is made by the following method: taking the bletilla striata, the sorbierite that 4~6 times of weight of bletilla striata weight are added is water-soluble Liquid impregnates 0.5~1h, 2~3h of heating and refluxing extraction, filtering, and filter vacuum is concentrated under reduced pressure into the 1/5~1/6 of original volume, is made Bletilla striata extract;In the sorbitol aqueous solution, the weight ratio of sorb alcohol and water is 1:(2~4).
2. anti-calculus dentalis Chinese medicinal toothpaste as described in claim 1, which is characterized in that by the raw material preparation of following parts by weight meter At: 6 parts of Chinese medicine, 0.2 part of saccharin sodium, 0.08 part of tertiary sodium phosphate, 4 parts of glycerol, 50 parts of sorbierite, 0.6 part of titanium dioxide, carragheen 0.4 part, it is 0.8 part of carboxymethyl cellulose, 13 parts of silicon 201A, 302 6 parts of silicon, 103 6 parts of silicon, 3 parts of lauryl sodium sulfate, thin 0.3 part of lotus brain, 0.1 part of menthyl lactate, 0.5 part of freshener WS-23,0.1 part of methylparaben, 0.1 part of ethylparaben and 20 parts of water;The Chinese medicine is made of bletilla striata extract, pearl shell powder and borneol according to weight ratio 4:1:2.
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WO2022109261A3 (en) * 2020-11-20 2022-07-21 Howard Frysh Dental calculus removal

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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
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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

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