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CN115463041B - Anti-sensitivity toothpaste with cold light whitening effect and preparation method thereof - Google Patents

Anti-sensitivity toothpaste with cold light whitening effect and preparation method thereof Download PDF

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CN115463041B
CN115463041B CN202211193120.9A CN202211193120A CN115463041B CN 115463041 B CN115463041 B CN 115463041B CN 202211193120 A CN202211193120 A CN 202211193120A CN 115463041 B CN115463041 B CN 115463041B
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toothpaste
parts
peroxide
mixture
titanium dioxide
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CN115463041A (en
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唐伟月
张环
董海德
邓全富
赵爽
卢静
陆瑜
邓嵘
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Chongqing Dencare Corp
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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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25Silicon; Compounds thereof
    • 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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/22Peroxides; Oxygen; Ozone
    • 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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • 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
    • 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
    • A61K8/39Derivatives containing from 2 to 10 oxyalkylene groups
    • 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
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • 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
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30Characterized by the absence of a particular group of ingredients
    • A61K2800/31Anhydrous
    • 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
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The application relates to the technical field of oral care products, in particular to anti-sensitivity toothpaste with a cold light whitening effect and a preparation method thereof. The toothpaste comprises bioactive glass ceramic material, peroxide and titanium dioxide. When brushing teeth, peroxide is contacted with water in the oral cavity to hydrolyze to form hydrogen peroxide, and under the condition that titanium dioxide is used as a catalyst, active oxygen is released by oxidation reaction, penetrates through enamel and dentin and reacts with pigment groups to be decomposed into small molecules to be emitted to the surface of teeth, so that the tooth color is changed to realize tooth whitening. Meanwhile, the bioactive glass ceramic material added in the formula can rapidly deposit bone-like apatite in the tooth brushing process, and has the effects of relieving and alleviating the tooth sensitivity after bleaching and promoting the remineralization of the tooth surface. Therefore, the toothpaste solves the problems of difficult storage of peroxide, easy tooth sensitivity caused by cold light whitening and the like, and has wide application prospect.

Description

Anti-sensitivity toothpaste with cold light whitening effect and preparation method thereof
Technical Field
The application relates to the technical field of oral care products, in particular to anti-sensitivity toothpaste with a cold light whitening effect and a preparation method thereof.
Background
Toothpaste is one of daily necessities, and is an oral care product for cleaning teeth, refreshing breath and being safe to human body. The learner survey showed that: 55.1% of the individuals are not satisfied with the color of their own teeth, and nearly 50% of the individuals wish to be able to make their own teeth beautiful and to improve their own appearance and quality. For whitening teeth, the tooth whitening toothpaste on the market at present mainly removes stains on the surface of teeth through physical cleaning of a friction agent, a dental calculus inhibitor (polyphosphate and the like) prevents deposition of colored groups, inhibits dental calculus formation, and calcium phosphate deposits on the surface of teeth to prevent bacteria from forming dental plaque.
Luminescence whitening teeth is a kind of room bleaching by means of luminescence LED lamps, and usually a bleaching material with high concentration of peroxide as a main component is coated on the surface of dyed teeth, and luminescence irradiation is given. The whitening cream has the advantages of short whitening time, obvious curative effect and the like, and is widely applied. The peroxide is used for whitening gel and tooth paste to whiten teeth, and the whitening effect is also confirmed by consumers. Because of its unstable chemical properties, it is difficult to popularize in conventional toothpastes despite its outstanding effect. The shelf life of toothpaste is typically three years longer than the shelf life of gel products, and some of the commonly used materials in toothpaste formulations are also less compatible with peroxides. Thus, commercial toothpastes have few peroxide components present due to the difficulty in maintaining paste stability. In addition, about 84.6% of the population bleaching teeth with bleaching agents is exposed to tooth sensitivity, while the enamel surface is rough and the gums are eroded by peroxide. The toothpaste in the prior art is also difficult to organically combine the cold light whitening function and the anti-sensitive function, and is difficult to meet the market demand.
Disclosure of Invention
The application aims to provide anti-sensitive toothpaste with cold light whitening effect, so as to solve the technical problem that toothpaste with cold light whitening and anti-sensitive effects and good stability is lacking in the prior art.
In order to achieve the above purpose, the application adopts the following technical scheme:
an anti-sensitive toothpaste with cold light whitening effect comprises bioactive glass ceramic material, peroxide and titanium dioxide, and no water.
The scheme also provides a preparation method of the anti-sensitive toothpaste with the cold light whitening effect, which comprises the following steps in sequence:
s1: mixing and dispersing a thickener carbomer and a part of friction agent to obtain a first mixture;
s2: mixing glycerol with the first mixture, and homogenizing to obtain a second mixture;
s3: mixing and homogenizing the second mixture with PEG-8 to obtain a third mixture;
s4: sequentially adding sweetener, bioactive glass ceramic material, peroxide, titanium dioxide and residual friction agent into the third mixture, mixing and homogenizing to obtain a fourth mixture;
s5: adding surfactant and essence into the fourth mixture, mixing, homogenizing, and vacuum degassing to obtain toothpaste.
The principle and the advantages of the scheme are as follows:
peroxide has poor long-term stability in conventional toothpaste, and is easy to release active oxygen to generate unstable phenomena such as toothpaste flatulence, etc., and the active oxygen is the key of oxidizing and decomposing tooth pigment. In addition, high concentrations of peroxide are prone to adverse reactions such as enamel demineralization, tooth sensitivity, gum irritation, etc. The inventor has conducted a great deal of research on toothpaste ingredients, and found that the anhydrous toothpaste formula can maintain the long-term stability of peroxide in the three-year shelf life of the toothpaste, active oxygen can exist in the toothpaste for a long time and keep activity, and the peroxide can be relatively stable ingredients with chemical properties such as calcium peroxide, carbamide peroxide, magnesium peroxide and the like. The low-concentration peroxide with micron-sized titanium dioxide as the catalyst is added into the toothpaste formula, and the toothpaste has excellent whitening effect on teeth under the irradiation of a cold light LED lamp. Peroxide is not easy to decompose under the sealing condition of toothpaste, and is hydrolyzed by contacting with water in oral cavity during brushingHydrogen peroxide (H) 2 O 2 ) The oxidation reaction is carried out to release active oxygen (superoxide ion free radical and hydroxyl free radical) to penetrate the enamel and dentin, and the active oxygen reacts with pigment groups to be decomposed into small molecules to be emitted to the surface of teeth, so that the color of the teeth is changed to realize tooth whitening. The maximum allowable use concentration of peroxide in toothpaste is not more than 3.0% (H in presence or release 2 O 2 Based on the weight of the tooth whitening composition), adverse reactions in the tooth whitening process can be remarkably reduced. Titanium dioxide as a catalyst has the same effect of whitening teeth as a low-concentration hydrogen peroxide mixture under a cold light LED light source. Meanwhile, the bioactive glass ceramic material added in the formula can rapidly deposit bone-like apatite in the tooth brushing process, and has the effects of relieving and alleviating the tooth sensitivity after bleaching and promoting the remineralization of the tooth surface.
In addition, the inventors have unexpectedly found that the combination of bioactive glass-ceramic materials with peroxide and titanium dioxide forms a whitening system that, in addition to providing relief from sensitivity to teeth after whitening, increases the whitening effect. The inventors analyzed that the reason may be that the bioactive glass-ceramic material may fill the small holes created by the use of peroxide, allowing the light to reflect and appear whiter.
In conclusion, the technical problem that the active oxygen of the peroxide-containing toothpaste in the prior art is unstable in the shelf life is solved, the whitening effect of the active oxygen in the tooth whitening process is improved, and the tooth sensitivity phenomenon after the peroxide whitening teeth is relieved and lightened.
Further, peroxide is reacted with H 2 O 2 The mass ratio of the bioactive glass ceramic material to the peroxide to the titanium dioxide is 5-15:0.5-3:0.15-1.0. Within the dosage range, the bioactive glass ceramic material can realize the ideal dentin-anti-sensitivity effect, and the whitening system consisting of peroxide and titanium dioxide can realize the ideal dentin-anti-sensitivity effect. And, within the above ratio range, the bioactive glass ceramic material and the whitening system have synergistic whitening effectAnd the synergistic effect is achieved.
Further, the bioactive glass ceramic material is Na 2 O-CaO-SrO-SiO 2 -P 2 O 5 -an F system; the Na is calculated in parts by weight 2 O-CaO-SrO-SiO 2 -P 2 O 5 the-F system comprises SiO 2 12-45 parts, P 2 O 5 10-35 parts of CaO, 25-48 parts of Na 2 5-15 parts of O, 3.5-4.9 parts of SrO and 1.5-2.1 parts of F.
By adopting the technical scheme, after the bioactive glass ceramic material is added, mineral ions such as calcium, phosphate radical and the like can be released during tooth brushing, and the mineral ions are deposited on the surface of the opening of the dentin tubule to form hydroxyapatite crystals so as to block the orifice. Meanwhile, the bioglass with silicon dioxide as a main network is hydrolyzed to form a gel film which can adsorb calcium and phosphorus ions and prevent the calcium and phosphorus ions from desolventizing in dentinal tubules, so that defect repair is accelerated and dentin sensitivity resistance is realized. Na (Na) 2 O-CaO-SrO-SiO 2 -P 2 O 5 The preparation of the F system can be seen in the applicant's prior patent CN103449725B (a bioactive glass ceramic material, its preparation and its use in oral care products).
Further, the peroxide includes at least one of carbamide peroxide, calcium peroxide and magnesium peroxide. Urea peroxide, calcium peroxide, and magnesium peroxide all provide hydrogen peroxide and have better stability relative to hydrogen peroxide in an anhydrous environment.
Further, the peroxide is calcium peroxide.
By adopting the technical scheme, the effect of the calcium peroxide is better than that of carbamide peroxide and magnesium peroxide, and the main appearance is that: magnesium peroxide has a certain risk of reacting with some raw material components of the toothpaste to cause certain problems of stability of the toothpaste; the carbamide peroxide has larger molecular weight, the hydrogen peroxide generating efficiency is lower, compared with calcium peroxide and magnesium peroxide, the same hydrogen peroxide yield can be obtained by larger addition amount, and the substance is easy to bring bad revenues to consumers; more importantly, the whitening effect of the calcium peroxide is more remarkable under the same theoretical release amount of hydrogen peroxide and the same amount of the bioactive glass ceramic material.
The calcium peroxide is used as a stable active oxygen providing agent, the hydrogen peroxide provided by the peroxide in the same mass part is more, the self stability is better, and the bioactive ceramic itself contains the calcium element and does not bring about the introduction of other additional substances.
Further, the crystalline form of titanium dioxide comprises anatase and/or rutile.
By adopting the technical scheme, the titanium dioxide can be used as a catalyst to accelerate the release of hydrogen peroxide, and the mass fraction of the titanium dioxide is generally maintained to be 0.15% -1.0%, so that the white appearance and taste of the paste are not affected while the release of the hydrogen peroxide is promoted. When the titanium dioxide content is lower than 0.15%, the appearance of the paste is semitransparent and milky and affects the appearance; when the titanium dioxide content is higher than 1.0%, there is a bitter taste affecting the paste taste.
Further, the material comprises the following raw materials in parts by weight: 5 to 35 parts of abrasive, 0.6 to 1.3 parts of thickener, 48 to 76 parts of humectant, 1.4 to 2.5 parts of surfactant, 0.1 to 0.25 part of sweetener and 0.8 to 1.2 parts of essence. The raw materials are conventional additive components of toothpaste.
Further, the humectant comprises at least one of glycerin, PEG-6, and PEG-8; the abrasive comprises calcium carbonate and/or hydrated silica; the thickener is carbomer; the surfactant is sodium lauryl sulfate.
By adopting the technical scheme, the carbomer is used as the thickener, the slivering property of the whole paste can be maintained in an anhydrous environment, and meanwhile, the carbomer can improve the residence of an active substance in an oral cavity and enhance the anti-sensitivity effect of the bioactive glass ceramic material.
Further, the humectant is 40-60 in mass ratio: 8-16 glycerol and PEG-8; the mass ratio of the friction agent is 0-20:5-15 of calcium carbonate and hydrated silica. The proportion of the friction agent can ensure better tooth cleaning effect. In the preparation of toothpastes containing bioactive glass-ceramic materials, peroxides and titanium dioxide, the inventors have found that the choice of humectant type is important for maintaining paste morphology. Glycerin is a necessary humectant, and the amount of glycerin needs to be maintained above a certain level to better maintain the stability of the toothpaste body so as to meet the quality requirements of related products.
Detailed Description
The present application will be described in further detail with reference to examples, but embodiments of the present application are not limited thereto. Unless otherwise indicated, the technical means used in the following examples and experimental examples are conventional means well known to those skilled in the art, and the materials, reagents and the like used are all commercially available.
The general situation of the technical scheme is as follows:
the anti-sensitivity toothpaste with the cold light whitening effect comprises the following raw material components in parts by weight: 5-35 parts of abrasive, 5-15 parts of bioactive glass ceramic material, peroxide (released H 2 O 2 Calculated by weight) 0.5-3.0 parts, 0.15-1.0 parts of titanium dioxide, 0.6-1.3 parts of thickening agent, 48-76 parts of humectant, 1.4-2.5 parts of surfactant, 0.1-0.25 parts of sweetener and 0.8-1.2 parts of essence.
The bioactive glass ceramic material belongs to Na 2 O-CaO-SrO-SiO 2 -P 2 O 5 F system, the synthesis of which is described in the applicant's prior patent CN103449725B (a bioactive glass-ceramic material, its preparation and its use in oral care products). The peroxide comprises at least one of calcium peroxide, magnesium peroxide and carbamide peroxide, preferably calcium peroxide. The humectant is at least one of glycerol, PEG-6 and PEG-8, and as a preferable technical scheme, the humectant is a combination of glycerol and PEG-8; the mass ratio of the glycerol to the PEG-8 is 40-60:8-16 (i.e., the mass ratio of glycerin to PEG-8 is in the range of 2.5-7.5), the humectant is preferably used in an amount in the range of 48.1-75.2. The friction agent is a mixture of calcium carbonate and hydrated silicon dioxide, the dosage range of the friction agent is preferably 15-27 parts, more preferably 15-25 parts, and the mass ratio of the calcium carbonate to the hydrated silicon dioxide is 0-20:5-15. The thickener is carbomerAs a preferred embodiment, the carbomer model is 956. The crystal form of the titanium dioxide is at least one of anatase and rutile, the titanium dioxide used in the technical scheme accords with GB 27599-2011 titanium dioxide for cosmetics, and the standard specifies that the titanium dioxide fineness is less than 45 mu m and accounts for 0.1% by mass, and the particle size distribution is 10-400 mu m. As a preferred technical scheme, the titanium dioxide crystal form is anatase, and the titanium dioxide crystal forms in the following examples and comparative examples are anatase. The surfactant is sodium lauryl sulfate. The sweetener comprises at least one of sodium saccharin and sucralose. The essence can be peppermint, menthol, etc.
According to the formula, the method for preparing the anti-sensitive toothpaste with cold light whitening effect comprises the following steps:
(1) Dispersing and mixing thickener carbomer and partial friction agent silicon dioxide (about 1-3% of formula amount of hydrated silicon dioxide, and 3% of the dosage is specifically used in examples and comparative examples) to obtain a first mixture for later use;
(2) Adding glycerol into a dissolver, then adding the first mixture, mixing humectant glycerol with the first mixture, and stirring uniformly to obtain a second mixture;
(3) Adding the remaining humectant PEG-8 into the second mixture, and uniformly stirring to obtain a third mixture;
(4) Sequentially adding sweetener, bioactive glass ceramic material, peroxide, titanium dioxide and the rest friction agent into the third mixture, and uniformly stirring to obtain a fourth mixture;
(5) And adding a surfactant and essence into the fourth mixture, homogenizing and stirring, and vacuum degassing to obtain the ointment.
Examples and comparative examples
The scheme of the application will now be illustrated and verified by means of specific examples and comparative examples, which are given below: examples 1-6, comparative examples 1-15 were formulated according to the protocol described above, and the formulations of examples 1-6, comparative examples 1-15 are detailed in tables 1-4. For ease of comparison, the biopsies used in examples and comparative examplesThe glass ceramic materials were obtained according to the preparation method of group II of example 1 of the previous patent CN 103449725B. Na obtained by the preparation method of all bioactive glass ceramic materials described in CN103449725B 2 O-CaO-SrO-SiO 2 -P 2 O 5 The F system bioactive ceramics can be used in the toothpaste manufacture of the scheme, and can generate antiallergic effect and synergistic whitening effect with peroxide. In examples 1 to 6, the mass fraction of peroxide was converted to the mass fraction of hydrogen peroxide produced, and was 0.5 part, 3 parts, and 3 parts, respectively.
Table 1: examples 1 to 6 technical parameters
Table 2: comparative examples 1 to 5 technical parameters
Table 3: comparative examples 6 to 10 technical parameters
Table 4: comparative examples 11 to 15 technical parameters
Experimental example 1: stability observation of anti-sensitive toothpaste body with cold light whitening effect
Stability observations were made for examples and comparative examples at room temperature and 45 c, with reference to GB 8372-2017 toothpaste. The experimental results are shown in tables 5 and 6. The toothpaste pastes prepared in examples 1-6 were stable. According to the observation results of comparative examples 1 to 6 and comparative examples 1 and 2, the anti-sensitive toothpaste with cold light whitening effect uses carbomer as a thickener, and when the mass fraction is 0.6% -1.3%, the appearance quality stability of the paste is normal, the slivers are good, and the phenomenon of abnormal increase of consistency is avoided. According to the observation results of comparative examples 3 and 4, when the anti-sensitive toothpaste with cold light whitening effect uses unsuitable humectant or surfactant, the stability of the appearance quality of the paste is normal in the early stage, and unstable phenomena such as flatulence, moisture and the like still occur in the later stage. The inventors analyzed that the reason is that sorbitol and N-acyl sarcosinate introduce moisture, which affects the moisture content of the toothpaste as a whole, resulting in unstable paste. Therefore, in preparing the toothpaste of the present embodiment, a suitable humectant (glycerin and PEG-8) and surfactant (sodium lauryl sulfate) are selected to obtain a toothpaste with satisfactory stability.
In comparative example 12, propylene glycol, a common humectant, was used in place of glycerin, but the toothpaste was thinner. In comparative example 13, the amount of glycerol used was relatively low, lower than that of glycerol and PEG-8=40-60: 8-16, but toothpaste is thinner. This demonstrates that in a toothpaste containing bioactive ceramic + peroxide + titanium dioxide, proper humectant is important for maintaining paste stability, glycerin is the humectant that must be used, and the amount of glycerin needs to be maintained above a certain level to better maintain stability of the toothpaste paste, so as to meet the relevant product quality requirements.
Comparative example 7 used hydrogen peroxide, which is itself unstable, typically an aqueous solution, and affects paste stability for anhydrous formulations. In example 4, magnesium peroxide was used, which had some reaction with other ingredients in the toothpaste, resulting in hard paste and hard extrusion during the experiment.
In comparative example 5, a semitransparent state occurs at a high temperature when the titanium dioxide content is too low, and the titanium dioxide acts as a light-shielding agent, and the titanium dioxide content is too low to completely cover the paste (itself is transparent), and only a part of the covered paste is milky white, while a part of the uncovered paste is still transparent, and a semitransparent state occurs. Comparative example 11 does not contain titanium dioxide, and shows a state of a transparent paste at a high temperature.
Table 5: the observation record of the appearance stability of the paste (the left side is room temperature test result, the right side is 45 ℃ test result; if the test results are the same in both cases, the record is not repeated, the paste is not striped after being extruded from the toothpaste, the paste cannot maintain the striped shape and collapse occurs, the paste is thinner, the paste has low viscosity and is difficult to form, the paste is more similar to fluid (thinner) than the paste in the case of 'no striping', the hardness and the hardness are both that the paste viscosity is increased, the hardness is slightly increased, the paste viscosity is hardened, and the paste viscosity is more than 300 pa.s
Table 6: paste appearance abnormality observation record
Experimental example 2: anti-sensitivity toothpaste body cold light whitening effect evaluation method with cold light whitening effect
The experiment is carried out by taking bleached and discolored bovine anterior teeth as a model. Bovine anterior model treatment was performed in reference (influence of different light sources of different antiallergic agents on tooth bleaching effect by hydrogen peroxide and titanium dioxide concentrations), and the specific method is: thawing frozen bovine front teeth, cutting root crowns and removing dental pulp, and treating with hypochlorous acid solution for 1 min. After washing with tap water and drying for 1 minute, the gel was treated with phosphoric acid for 1 minute. Re-washed with tap water and dried. Then soaking in black tea boiled in boiling water for seven days to generate color-changing specimens, testing by adopting toothpaste groups passing through paste stability test, wherein each toothpaste group adopts 5 specimens (n=5), the degree of color level elevation is averaged, and each test tooth is the same color level (A4) so as to ensure the parallelism of the experiment. Comparative examples 9 to 15 in the experiment performed with reference example 1 at normal temperature, the pastes were all normal, and in the subsequent study, it was noted that the efficacy test was performed by the stability test (efficacy experiment of whitening effect was performed at normal temperature). However, in practical application (product use), the paste characteristics deviate from normal in a stability experiment at 45 ℃ of the product, so that user experience is affected, and the paste needs to be avoided as much as possible.
The specimen is wetted in artificial saliva, the toothpaste prepared in the examples and comparative examples is uniformly smeared on the stained enamel surface (the thickness of the toothpaste smeared on the tooth surface is about 2-3mm, no additional water is added into the paste because the model is in a wetted state), and the toothpaste is irradiated by an LED lamp with the wavelength of 365+/-10 nm from the tooth surface at a distance of 1 cm. After 1h of irradiation of the enamel surface, the teeth were removed and washed, and the whitening effect was evaluated colorimetrically using a dental professional 16-color palette. Tooth color chart is a standard for tooth whitening. The color level of the teeth is compared before the teeth are whitened, and the teeth are whitened and then compared once. The scheme uses a vitamin A (VITA) color chart, which is a common evaluation tool in the cold light whitening process. The english letters on the vitamin a color chart represent the color propensity of tooth staining. The 16 color chart is arranged from left to right from shallow to deep: 1- > B1, 2- > A1, 3- > B2, 4- > D2, 5- > A2, 6- > C1, 7- > C2, 8- > D3, 9- > A3, 10- > D4, 11- > B3, 12- > A3.5, 13- > B4, 14- > C3, 15- > A4, 16- > C4. In the above letters: a represents reddish brown; b represents red-yellow; c represents gray; d represents red gray. The numbers following the letters then represent the degree of staining of the teeth: the higher the number, the greater the degree of color cast. The experimental results are shown in table 7. Based on the observations of the comparative examples and comparative examples, the anti-sensitive toothpaste having luminescence whitening effect uses peroxide with a mass fraction of 0.5% -3.0% (H present or released) 2 O 2 Calculated), the ointment has the whitening effect.
Table 7: evaluation, observation and record of paste luminescence whitening effect
Toothpaste group Degree of tone step elevation (average value) Toothpaste group Degree of tone step elevation (average value)
Example 1 1.0 Comparative example 8 0.4
Example 2 4.0 Comparative example 9 0.6
Example 3 2.2 Comparative example 10 2.2
Example 4 3.2 Comparative example 11 0
Example 5 3.2 Comparative example 12 1.2
Example 6 3.0 Comparative example 13 1.0
Comparative example 6 1.0 Comparative example 14 2.8
/ / Comparative example 15 0.2
From the experimental data in table 7, we can understand the synergistic effect of bioactive glass-ceramic materials and whitening systems (peroxide and titanium dioxide) from example 1, comparative example 9 and comparative example 11. Comparative example 9 used only whitening system (1.05 parts of calcium peroxide + 0.15 parts of titanium dioxide), comparative example 11 used only bioactive glass ceramic material (5 parts of ceramic material), and example 1 used both (5 parts of ceramic material + 1.05 parts of calcium peroxide + 0.15 parts of titanium dioxide). Example 1 increased the tooth level by 1.0, while comparative example 9 and comparative example 11 did not all show the level-increasing effect. The inventors speculate that the whitening effect of the toothpaste is improved due to the synergistic effect between the bioactive glass ceramic material and the whitening system. We can also see from example 2, comparative example 14 and comparative example 15 that the synergy of the bioactive glass-ceramic material and the whitening system is still present in the case of increasing the content of both. Comparative example 14 used only whitening system (6.35 parts of calcium peroxide + 1 part of titanium dioxide), comparative example 15 used only bioactive glass ceramic material (15 parts of ceramic material), and example 2 used both (15 parts of ceramic material + 6.35 parts of calcium peroxide + 1 part of titanium dioxide). Example 2 the average of the tooth color levels of the whitening effect was increased by 4.0, comparative example 14 was increased by only 2.8 color levels, comparative example 15 did not use the whitening system, hardly any whitening effect was achieved, and the average of the increased color levels was 0.2 (the presence of a synergy was demonstrated by comparing example 2, comparative example 14 and comparative example 15).
Examples 4 and 5 use different hydrogen peroxide providing substances relative to example 2, and in three examples the amount of hydrogen peroxide theoretically produced is consistent. However, the toothpastes of examples 4 and 5 were inferior in whitening effect to the toothpaste of example 2. This shows that the effect of using calcium peroxide is better than that of carbamide peroxide and magnesium peroxide in whitening effect, and is more suitable for preparing whitening anti-allergic toothpaste.
Experimental example 3: anti-sensitive toothpaste with cold light whitening effect and observation of dentin sensitivity clinical effect
The experimental method comprises the following steps:
1. the subjects were healthy adult males and females who met inclusion and exclusion criteria. A total of 84 eligible subjects were enrolled in the baseline examination and 80 subjects completed the study for a total of 8 weeks.
2. Inclusion criteria: age between 18-70 years old; the whole body health condition is good; the test can be attended on time within 8 weeks of the test; in the case of females, it is not necessary to be in gestation and lactation; at least 1 tooth with dentin sensitivity is a bicuspid tooth or an anterior tooth, the neck of the tooth is worn or the neck gingiva is retracted, and the following conditions are satisfied: the probe inspection (Yeaple probe) is sensitive to 10-30g of touch stimulus, and/or the cold air stimulus count value is more than or equal to 2; the toothpaste and the components thereof are not allergic; willing to take part in the trial and sign informed consent; no following drugs were allowed for the current 1 month of participation in this study: anticonvulsants, antihistamines, antidepressants, sedatives, tranquilizers; no other anti-sensitivity toothpaste was used for the current 3 months of participation in the study; other similar experimental studies were not concurrently enrolled.
The experimental results are shown in tables 8-11, and at the time of baseline examination, there is no statistical difference between the detection values of the cold air blowing sensitivity index and the detection values of the control group (the bioactive glass ceramic material, the peroxide and the titanium dioxide are omitted on the basis of the formula of the example 1). After 2 weeks of toothpaste application, the cold air jet sensitivity index of the subject of example 1 gradually decreased, while the probe sensitivity index gradually increased, all with statistical differences from its baseline value; suggesting that there is some dentinal sensitivity alleviating effect starting after two weeks of use of example 1. After weeks 2, 4, 6, and 8 of toothpaste application, the cool air blowing sensitivity index of example 1 group decreased and the probe sensitivity index increased, all statistically different from the control group. Demonstrating that example 1 has a more pronounced effect on improving dentinal sensitivity symptoms than the control group under the conditions of the study. While example 1 contained peroxide which had a negative effect on dentinal sensitivity, the use of bioactive glass ceramic material in this embodiment counteracts dentinal sensitivity due to peroxide, and the toothpaste of example 1 had a better anti-sensitivity effect than the control group without peroxide.
Table 8: summary of evaluation of the sensitivity of detection
a: within the same test toothpaste group, the comparison of different time points with the baseline value of the group has statistical significance;
b: at the same time point, the method has statistical significance compared with the control group.
Table 9: example 1 percent increase in detection sensitivity over control toothpaste group
Percent= (test group-control group)/control group 100%; * At the same time point, has statistical significance compared with the control group
Table 10: summary of cool air blowing sensitivity evaluation
a: within the same test toothpaste group, the comparison of different time points with the baseline value of the group has statistical significance;
b: at the same time point, the method has statistical significance compared with the control group.
Table 11: example 1 toothpaste set was changed from control set in cold air blow test value
Percent= (test group-control group)/control group 100%; * At the same time point, has statistical significance compared with the control group
The foregoing is merely exemplary of the present application, and specific technical solutions and/or features that are well known in the art have not been described in detail herein. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present application, and these should also be regarded as the protection scope of the present application, which does not affect the effect of the implementation of the present application and the practical applicability of the patent. The protection scope of the present application is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.

Claims (5)

1. An anti-sensitive toothpaste with cold light whitening effect is characterized in that: the raw materials comprise bioactive glass ceramic materials, calcium peroxide, titanium dioxide and a humectant, and the raw materials do not comprise water;
peroxide in H 2 O 2 The mass ratio of the bioactive glass ceramic material to the calcium peroxide to the titanium dioxide is 5-15:0.5-3:0.15-1.0;
the raw materials also comprise 5 to 35 parts of abradant, 0.6 to 1.3 parts of thickener, 48 to 76 parts of humectant, 1.4 to 2.5 parts of surfactant, 0.1 to 0.25 part of sweetener and 0.8 to 1.2 parts of essence;
the bioactive glass ceramic material is Na 2 O-CaO-SrO-SiO 2 -P 2 O 5 -F systemThe method comprises the steps of carrying out a first treatment on the surface of the The Na is calculated in parts by weight 2 O-CaO-SrO-SiO 2 -P 2 O 5 the-F system comprises SiO 2 12-45 parts, P 2 O 5 10-35 parts of CaO, 25-48 parts of Na 2 5-15 parts of O, 3.5-4.9 parts of SrO and 1.5-2.1 parts of F;
the humectant comprises the following components in percentage by mass: 8-16 glycerol and PEG-8; the thickener is carbomer; the surfactant is sodium lauryl sulfate.
2. An anti-sensitivity toothpaste with cold light whitening effect according to claim 1, wherein: the crystalline form of titanium dioxide comprises anatase and/or rutile.
3. An anti-sensitivity toothpaste with luminescent whitening effect according to claim 2, wherein said abrasive comprises calcium carbonate and/or hydrated silica.
4. An anti-sensitive toothpaste with cold light whitening effect according to claim 3, wherein said abrasive is 0-20 by mass: 5-15 of calcium carbonate and hydrated silica.
5. The method for preparing the anti-sensitivity toothpaste with cold light whitening effect according to claim 4, wherein the method comprises the following steps: the method comprises the following steps of:
s1: mixing and dispersing a thickener carbomer and a part of friction agent to obtain a first mixture;
s2: mixing glycerol with the first mixture, and homogenizing to obtain a second mixture;
s3: mixing and homogenizing the second mixture with PEG-8 to obtain a third mixture;
s4: sequentially adding sweetener, bioactive glass ceramic material, peroxide, titanium dioxide and residual friction agent into the third mixture, mixing and homogenizing to obtain a fourth mixture;
s5: adding surfactant and essence into the fourth mixture, mixing, homogenizing, and vacuum degassing to obtain toothpaste.
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