CN115708799B - Mild caries-preventing children liquid toothpaste and preparation method thereof - Google Patents
Mild caries-preventing children liquid toothpaste and preparation method thereof Download PDFInfo
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- CN115708799B CN115708799B CN202211625065.6A CN202211625065A CN115708799B CN 115708799 B CN115708799 B CN 115708799B CN 202211625065 A CN202211625065 A CN 202211625065A CN 115708799 B CN115708799 B CN 115708799B
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- 230000007774 longterm Effects 0.000 description 1
- 235000010335 lysozyme Nutrition 0.000 description 1
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- 230000019612 pigmentation Effects 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
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- 239000005017 polysaccharide Substances 0.000 description 1
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- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
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Abstract
The invention relates to a mild caries-preventing children liquid toothpaste and a preparation method thereof, wherein the toothpaste comprises the following components in percentage by weight: 0.5 to 2.0 percent of cinnamic acid modified chitosan nano-particles, 0.01 to 2.0 percent of compound amino acid composition, 0.01 to 2.0 percent of lactobacillus paracasei ADP-1, 1.0 to 3.0 percent of foaming agent, 0.1 to 0.5 percent of thickening agent, 50 to 70 percent of humectant, 8.0 to 15.0 percent of silicon dioxide, 0.2 to 0.5 percent of sodium benzoate and the balance of deionized water.
Description
Technical Field
The invention relates to the field of daily chemical cleaning products, in particular to a mild caries-preventing liquid toothpaste for children and a preparation method thereof.
Background
Caries is a caries lesion of hard tissues of teeth, which is mainly represented by mineral demineralization and organic decomposition of teeth to form cavities, due to the adhesion of cariogenic food sugar (particularly sucrose and refined carbohydrate) to the tooth surface, and the formation of an acquired film from salivary proteins, which can not only be firmly adhered to the tooth surface, but also be decomposed by cariogenic bacteria in the oral cavity at a proper temperature to generate acids, which attack the teeth. One of the important means for preventing caries is to brush teeth, and the cariogenic food sugar and the acquired film on the tooth surface are cleaned by the toothpaste and the toothbrush, so that the toothpaste plays an important role in protecting the health of gums and cleaning teeth.
The existing toothpaste is mainly used for preventing dental caries by adding plant extracts such as polyphenol, alkaloid, flavone and the like or bacteriostatic agents such as fluoride salt, phosphate, arsenic chloride and the like, has no obvious inhibition effect on cariogenic bacteria, and is easy to cause unbalanced flora in the oral cavity. For this reason, chinese patent application CN108324675a discloses a toothpaste containing lactobacillus paracasei, comprising 0.5 to 1% of sweetener, 0.05 to 0.1% of o-cymene-5-ol, 0.4 to 0.8% of sodium pyrophosphate, 10 to 15% of glycerin, 0.3 to 0.8% of sodium hydroxymethyl cellulose, 0.5 to 1% of xanthan gum, 35 to 50% of sorbitol, 5 to 10% of silica, 0.3 to 0.7% of colorant, 10 to 15% of dibasic calcium phosphate dihydrate, 2 to 3% of surfactant, 0.5 to 1% of lactobacillus paracasei, 0.8 to 1.5% of essence, and the balance being water, wherein by using o-cymene-5-ol and inactivated lactobacillus paracasei, the o-cymene-5-ol not only can effectively inhibit the influence of the metabolites of the inactivated lactobacillus paracasei on the paste, but also can cooperate with lactobacillus paracasei in use, thereby effectively inhibiting pathogenic bacteria in oral cavity. In addition, chinese patent application CN113832062A discloses a lactobacillus paracasei LC86 and application thereof in preventing or treating dental caries and periodontitis, which shows that the lactobacillus paracasei LC86 has strong inhibition capability to oral pathogenic bacteria streptococcus mutans, has high resistance to lysozyme, has strong self-aggregation capability and copolymerization capability with streptococcus mutans, can inhibit formation of pathogenic bacteria biomembrane, and shows that the strain can effectively reduce adhesion of pathogenic bacteria in oral cavity.
At present, the toothpaste containing antibacterial components or lactobacillus paracasei can only inhibit cariogenic bacteria in the oral cavity in a short time, so that the cariogenic bacteria are reduced, and the caries preventing effect is achieved, but the cariogenic bacteria are obviously reduced in a short time after tooth brushing, but the cariogenic bacteria are also increased along with the time, and the antibacterial components and the lactobacillus paracasei in the toothpaste are difficult to coexist, so that the caries preventing effect is required to be improved.
Disclosure of Invention
In order to solve the problems, the invention provides mild caries-preventing liquid toothpaste for children and a preparation method thereof.
The technical scheme adopted by the invention is that the mild caries-preventing children liquid toothpaste comprises the following components in percentage by weight: 0.5 to 2.0 percent of cinnamic acid modified chitosan nano particles, 0.01 to 2.0 percent of compound amino acid composition, 0.01 to 2.0 percent of lactobacillus paracasei ADP-1, 1.0 to 3.0 percent of foaming agent, 0.1 to 0.5 percent of thickening agent, 50 to 70 percent of humectant, 8.0 to 15.0 percent of silicon dioxide, 0.2 to 0.5 percent of sodium benzoate and the balance of deionized water.
The silicon dioxide is used as a friction agent, can act together with a toothbrush in the toothpaste to wipe off cariogenic food sugar and acquired films on the surfaces of teeth, reduces the formation of dental stains, dental plaque, dental calculus and the like, and has the addition ratio of 8.0-15.0%, so that the toothpaste has a low friction value and a low friction value to avoid wearing children teeth; the deionized water is a gel dispersion medium of the toothpaste; the lactobacillus paracasei ADP-1 is adhered with pathogenic bacteria in the oral cavity, and then the pathogenic bacteria are physically removed through tooth brushing, mouth rinsing and oral cavity movement, so that the effects of maintaining the teeth and the oral cavity are achieved; the compound amino acid composition can provide amino acids necessary for human body, promote human body development, enhance immunity, and improve central nervous tissue function.
Preferably, a mild anticarious child fluid dentifrice, further comprising at least one of the following adjuvants in weight percent: 0.01 to 2.0 percent of casein phosphopeptide, 0.01 to 2.0 percent of calcium glycerophosphate, 0.1 to 2.0 percent of xylitol, 0.5 to 0.7 percent of sodium monofluorophosphate, 0.5 to 1.2 percent of essence, 0.1 to 0.3 percent of sweetener, 0.2 to 0.5 percent of preservative and 0.1 to 1.0 percent of colorant.
Preferably, casein phosphopeptides (CPP) are bioactive polypeptides prepared from bovine casein as a raw material by biotechnology, wherein the CPP can promote calcium utilization of teeth and simultaneously stimulate salivary secretion, so that alkaline saliva can buffer acidic substances on dental plaque from corroding enamel, and dental caries can be prevented; the calcium glycerophosphate can enhance tooth calcium and has tooth whitening effect; the xylitol can not be fermented and utilized by bacteria producing dental caries in the oral cavity, can promote salivary secretion, slow down acidification of the oral cavity, and is helpful for preventing dental caries.
Preferably, the colorant is at least one of titanium dioxide and pigment, which gives the toothpaste a better appearance.
Preferably, the humectant is sorbitol and polyethylene glycol, which can maintain the moisture of the paste, maintain the fluidity of the paste and reduce the freezing point of the paste.
Preferably, the sweetener is sucralose, which masks the bad taste of the toothpaste and improves the mouthfeel of the toothpaste.
Preferably, the preservative is sodium benzoate, has good fermentation prevention, bacterial proliferation inhibition and sterilization capacity, and is a common preservative in toothpaste.
Preferably, the essence can be mint essence or fruit essence, and is used as an aroma-imparting agent in the toothpaste to endow the toothpaste with stable aroma and cool mouthfeel, mask the peculiar smell of the toothpaste ingredients and have antibacterial effect.
Preferably, the foaming agent is at least one of sodium lauryl glucose carboxylate, lauryl glucoside, sodium lauroyl glutamate, sodium methyl cocoyl taurate and cocamidopropyl betaine, has higher safety and low irritation, and can form fine and durable foam.
Preferably, the thickener is at least two of xanthan gum, carrageenan, cellulose gum and carbomer, and can suspend the solid phase of the toothpaste, prevent the solid phase component from being separated from the liquid phase component in the toothpaste, and simultaneously enable the toothpaste to have proper consistency so as to facilitate the extrusion of the toothpaste.
Preferably, the composite amino acid composition comprises the following components in percentage by weight: 50 to 80 percent of water, 1 to 10 percent of lysine, 1 to 10 percent of arginine, 1 to 10 percent of glycine, 1 to 10 percent of histidine, 0.5 to 1.0 percent of 1, 2-hexanediol and 0.2 to 1.0 percent of p-hydroxyacetophenone.
Preferably, the preparation method of the cinnamic acid modified chitosan nanoparticle comprises the following steps:
step 1: under the protection of argon, H is added into chitosan solution 2 O 2 Adding cinnamic acid into the solution and ascorbic acid, and carrying out oscillation reaction for 10-12 h at the temperature of 30-35 ℃; putting the reaction product into a dialysis bag of 12000-14000 Da for dialysis in deionized water, and finally, freeze-drying to obtain the cinnamic acid-chitosan graft copolymer;
step 2: dissolving cinnamic acid-chitosan graft copolymer in a citric acid buffer solution, preparing a CA-CTS solution with the concentration of 0.5-5%, and regulating the pH value to 5-5.9 for later use;
step 3: taking a pullulan sterilizing solution with the concentration of 0.5-2.0%, and carrying out centrifugal degassing treatment for later use; the rotational speed of the centrifugal degassing treatment is as follows: 2500-4500 r/min for 3-8 min;
step 4: mixing the CA-CTS solution with the pullulan sterilizing solution after pH adjustment according to the mass ratio of 1:1-8, adding the compound vitamin into the obtained mixed solution, then rapidly stirring for 1-3 h at 15-20 ℃, and carrying out atomization drying to obtain the cinnamic acid modified chitosan nano particles.
Preferably, in the step 1, the concentration of the chitosan solution is 1.0-5.0 g/L, H 2 O 2 The concentration of the solution is 1.0-2.0 g/L, the concentration of the ascorbic acid is 2-10 mg/L, chitosan solution and H 2 O 2 The volume ratio of the solution to the ascorbic acid is 1-5: 1 to 3: 1-2, and the molar ratio of cinnamic acid to chitosan is 3:1.
Preferably, in the step 4, the mass ratio of the mixed solution to the compound vitamin is 3-16:1, and the compound vitamin comprises at least one of the following components: vitamin D, vitamin K and vitamin C.
A preparation method of mild anticarious children liquid toothpaste comprises the following steps:
step 1: preparing a composite amino acid composition, adding the amino acid components into deionized water according to a proportion, fully stirring, adding 1, 2-hexanediol and p-hydroxyacetophenone while stirring, and stirring until the amino acid components are completely dissolved;
step 2: preparing a first composition, swelling the thickener, mixing humectant, foaming agent, sodium benzoate and water according to the weight percentage, stirring at 45-55 ℃, adding the thickener while stirring, stirring and dispersing uniformly until no mass exists, standing for 8-18 hours, and observing that the solution is uniform transparent thick liquid;
step 3: preparing a toothpaste composition, homogenizing, emulsifying and mixing a first composition, a composite amino acid composition, cinnamic acid modified chitosan nano particles, lactobacillus paracasei ADP-1 and an auxiliary agent according to a proportion;
step 4: adding the toothpaste composition into a paste making machine, adding silicon dioxide, stirring uniformly, simultaneously starting vacuum to remove bubbles, adding a foaming agent, mixing and stirring uniformly again, adjusting the pH to 6.8-7.2, homogenizing and emulsifying to obtain the liquid toothpaste.
The invention has the beneficial effects that:
caries is a common oral disease, the dental hard tissue injury is caused by the complex action of a plurality of factors, the manifestation is generally divided into mineral demineralization and organic decomposition, the process from color change to substantial lesion is progressed along with the disease course, the complexity of cariogenic factors determines that the caries prevention mode can not be started singly, and a plurality of components are needed to cooperate with each other so as to effectively prevent caries.
The sodium monofluorophosphate can inhibit the activities of various enzymes in the bacterial metabolic process to cause the growth metabolism to be disordered or stopped, and the lactobacillus paracasei ADP-1 and metabolites thereof can inhibit the adhesion of bacteria to tooth surfaces by being adhered with oral pathogenic bacteria, so that the combined action of the two can assist in the cleaning of the bacteria in the tooth brushing process while inhibiting the growth of caries pathogenic bacteria; the synergistic action mechanism of the calcium glycerophosphate and the casein phosphopeptide, the calcium glycerophosphate decomposes calcium ions in the oral cavity, and the casein phosphopeptide promotes the utilization of calcium by teeth and enhances the calcium quality of the teeth, thereby enhancing the acid resistance of the teeth; the compound amino acid composition is used as a nutrient substance, can promote the development of human bodies, is beneficial to the growth of teeth and gingiva, can not be used as nutrient by bacteria, can promote salivary secretion, slow down acidification of the oral cavity, and can realize the synergistic effect of tooth protection and bacteriostasis so as to achieve the effect of effectively preventing decayed teeth.
The mild caries preventing children liquid toothpaste contains cinnamic acid modified chitosan nano particles, can be retained in tooth gaps during tooth brushing, has certain antibacterial property and oxidation resistance, can effectively inhibit reproduction of streptococcus mutans and porphyromonas gingivalis, does not influence the activity of lactobacillus paracasei ADP-1, has DPPH free radical scavenging capability, can reduce the generation of an acquired film, prevent the oxidization of the acquired film and prevent the formation of dental jaundice, dental plaque and dental caries.
Drawings
The invention will be further described with reference to the accompanying drawings, in which embodiments do not constitute any limitation of the invention, and other drawings can be obtained by one of ordinary skill in the art without inventive effort from the following drawings.
FIG. 1 is a schematic representation of a colony of Streptococcus mutans CMCC32400 in a blank control group in a bacteriostasis test according to the present invention;
FIG. 2 is a schematic representation of the colony of Porphyromonas gingivalis ATCC 33277 in a blank control group in the antibacterial test of the present invention;
FIG. 3 is a schematic representation of the colony of Lactobacillus paracasei ADP-1 in a blank control group in the antibacterial test of the present invention;
FIG. 4 is a schematic representation of the colony of Streptococcus mutans CMCC32400 in a control group for the antibacterial test of the present invention;
FIG. 5 is a schematic representation of the colony of Porphyromonas gingivalis ATCC 33277 in the control group in the antibacterial test of the present invention;
FIG. 6 is a schematic representation of the colony of Lactobacillus paracasei ADP-1 in the control group in the antibacterial test of the present invention;
FIG. 7 is a schematic representation of the colony of Streptococcus mutans CMCC32400 in the test group of the antibacterial test of the present invention;
FIG. 8 is a schematic representation of the colony of Porphyromonas gingivalis ATCC 33277 in the test group of the antibacterial test of the present invention;
FIG. 9 is a schematic representation of the colony of Lactobacillus paracasei ADP-1 in the experimental group of the antibacterial test of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Unless otherwise specified, the raw materials used in the examples of the present invention were those conventionally commercially available in the art, and the equipment used was conventional equipment in the art.
Cinnamic acid: CAS No. 621-82-9, molecular formula: c (C) 9 H 8 O 2 The structural formula is as follows:
chitosan: CAS No. 9012-76-4, molecular formula (C) 6 H 11 NO 4 ) n has the structural formula:
pullulan polysaccharide: CAS No. 9057-02-7, molecular formula: c (C) 20 H 36 O 16 The structural formula is as follows:
the process and effect analysis of the cinnamic acid modified chitosan nanoparticle preparation method are as follows:
the invention uses cinnamic acid as raw material and passes H 2 O 2 Solutions and antigensThe oxidation-reduction system of the ascorbic acid initiates free radical induction reaction, cinnamic acid is grafted to the molecular chain of chitosan to form ester bond and amido bond to obtain modified chitosan, the crystallinity of the chitosan is obviously reduced by adding the cinnamic acid, the oxidation resistance is improved, the surface structure of the chitosan tends to be loose, and the DPPH free radical scavenging capability and the reducing capability of the modified chitosan are obviously higher than those of the unmodified chitosan;
modified chitosan molecules of-NH 3+ The compound vitamin is used for enhancing and regulating the absorption and excretion of calcium and phosphate by a human body, forming an extracellular ionic environment favorable for calcification of dental tissues, the vitamin K can protect teeth, promote the generation of dentin, even heal existing decayed teeth, prevent bacteria from generating acidic substances to corrode teeth, prevent periodontal diseases, reduce pigmentation and whiten teeth.
The invention is further described with reference to the following examples.
Example 1
A mild anticarious children liquid toothpaste comprises the following components in percentage by weight: 1.5% of cinnamic acid modified chitosan nano particles, 1% of composite amino acid composition, 0.8% of mint essence, 0.1% of lactobacillus paracasei ADP-1, 0.5% of sodium monofluorophosphate, 0.1% of casein phosphopeptide, 1.0% of calcium glycerophosphate, 1.0% of sodium lauryl glucose carboxylate, 1.0% of lauryl glucoside, 0.2% of xanthan gum, 0.2% of cellulose gum, 60% of sorbitol, 2% of polyethylene glycol, 12% of silicon dioxide, 0.2% of sucralose, 0.3% of sodium benzoate, 0.1% of titanium dioxide and the balance of deionized water; the compound amino acid composition comprises the following components in percentage by weight: 66.5% of water, 8% of lysine, 8% of arginine, 8% of glycine, 8% of histidine, 0.5% of 1, 2-hexanediol and 1% of p-hydroxyacetophenone.
The preparation method of the cinnamic acid modified chitosan nanoparticle comprises the following steps:
step 1: under the protection of argon, 1.0g/L H of chitosan solution with the concentration of 2.0g/L is added 2 O 2 Adding 5mg/L ascorbic acid into the solution, and adding cinnamic acid into the solution to react for 12 hours at 32 ℃ in an oscillating way; dialyzing the reaction product in 12000Da dialysis bag in deionized water, and lyophilizing to obtain cinnamic acid-chitosan graft copolymer, wherein chitosan solution and H 2 O 2 The volume ratio of the solution to the ascorbic acid is 3:2:1, the molar ratio of cinnamic acid to chitosan is 3:1;
step 2: dissolving cinnamic acid-chitosan graft copolymer in citric acid buffer solution, preparing CA-CTS solution with concentration of 4.0%, and regulating pH to 5 for use;
step 3: taking a pullulan sterilizing solution with the concentration of 1%, and carrying out centrifugal degassing treatment for later use; the rotational speed of the centrifugal degassing treatment is as follows: 3500r/min, time of 5min;
step 4: mixing the CA-CTS solution with the pullulan sterilizing solution after pH adjustment according to the mass ratio of 1:2, adding the compound vitamin into the obtained mixed solution, wherein the mass ratio of the mixed solution to the compound vitamin is 15:1, then rapidly stirring for 2 hours at 20 ℃, and carrying out atomization drying to obtain cinnamic acid modified chitosan nano particles; wherein the compound vitamin consists of vitamin D, vitamin K and vitamin C according to the mass ratio of 2:1:2.
A preparation method of mild anticarious children liquid toothpaste comprises the following steps:
step 1: preparing a composite amino acid composition, adding the amino acid components into deionized water according to a proportion, fully stirring, adding 1, 2-hexanediol and p-hydroxyacetophenone while stirring, and stirring until the amino acid components are completely dissolved;
step 2: preparing a first composition, swelling the thickener, mixing humectant, foaming agent, sodium benzoate and water according to weight percentage, stirring at 45deg.C, adding the thickener while stirring, stirring and dispersing uniformly until no lump exists, standing for 12 hr, and observing the solution to be uniform transparent thick liquid;
step 3: preparing a toothpaste composition, homogenizing, emulsifying and mixing a first composition, a composite amino acid composition, cinnamic acid modified chitosan nano particles, lactobacillus paracasei ADP-1 and an auxiliary agent according to a proportion;
step 4: adding the toothpaste composition into a paste making machine, adding silicon dioxide, stirring uniformly, simultaneously starting vacuum to remove bubbles, adding a foaming agent, mixing uniformly again, adjusting the pH value to 7.0, homogenizing and emulsifying to obtain the liquid toothpaste.
Example two
A mild anticarious children liquid toothpaste comprises the following components in percentage by weight: 2.0% of cinnamic acid modified chitosan nano particles, 1.0% of essence, 0.2% of lactobacillus paracasei ADP-1.2% of sodium monofluorophosphate, 0.05% of compound amino acid composition, 0.1% of xylitol, 1.5% of sodium methyl cocoyl taurate, 1.0% of sodium lauroyl glutamate, 0.25% of xanthan gum, 0.25% of carrageenan, 60% of sorbitol, 5% of polyethylene glycol, 10% of silicon dioxide, 0.3% of sucralose, 0.4% of sodium benzoate, 0.2% of colorant and the balance of deionized water; the compound amino acid composition comprises the following components in percentage by weight: 69.5% of water, 10% of lysine, 5% of arginine, 5% of glycine, 10% of histidine, 1, 2-hexanediol and 0.5% of p-hydroxyacetophenone.
The preparation method of the cinnamic acid modified chitosan nanoparticle comprises the following steps:
step 1: under the protection of argon, 2.0g/L H of chitosan solution with the concentration of 1.0g/L is added 2 O 2 Adding 10mg/L ascorbic acid into the solution, and adding cinnamic acid to react at 35 ℃ for 10 hours in an oscillating way; dialyzing the reaction product in 12000Da dialysis bag in deionized water, and lyophilizing to obtain cinnamic acid-chitosan graft copolymer, wherein chitosan solution and H 2 O 2 The volume ratio of the solution to the ascorbic acid is 5:1:1, the molar ratio of cinnamic acid to chitosan is 3:1;
step 2: dissolving cinnamic acid-chitosan graft copolymer in citric acid buffer solution, preparing CA-CTS solution with concentration of 3.0%, and regulating pH to 5 for use;
step 3: taking a pullulan sterilizing solution with the concentration of 1.5%, and carrying out centrifugal degassing treatment for later use; the rotational speed of the centrifugal degassing treatment is as follows: 4000r/min for 4min;
step 4: mixing the CA-CTS solution with the pullulan sterilizing solution after pH adjustment according to the mass ratio of 1:3, adding the compound vitamin into the obtained mixed solution, wherein the mass ratio of the mixed solution to the compound vitamin is 16:1, then rapidly stirring for 2.5 hours at 18 ℃, and carrying out atomization drying to obtain cinnamic acid modified chitosan nano particles; wherein the compound vitamin consists of vitamin D, vitamin K and vitamin C according to the mass ratio of 1:1:1.
A preparation method of mild anticarious children liquid toothpaste comprises the following steps:
step 1: preparing a composite amino acid composition, adding the amino acid components into deionized water according to a proportion, fully stirring, adding 1, 2-hexanediol and p-hydroxyacetophenone while stirring, and stirring until the amino acid components are completely dissolved;
step 2: preparing a first composition, swelling the thickener, mixing humectant, foaming agent, sodium benzoate and water according to weight percentage, stirring at 50deg.C, adding the thickener while stirring, stirring and dispersing uniformly until no lump exists, standing for 17 hr, and observing the solution to be uniform transparent thick liquid;
step 3: preparing a toothpaste composition, homogenizing, emulsifying and mixing a first composition, a composite amino acid composition, cinnamic acid modified chitosan nano particles, lactobacillus paracasei ADP-1 and an auxiliary agent according to a proportion;
step 4: adding the toothpaste composition into a paste making machine, adding silicon dioxide, stirring uniformly, simultaneously starting vacuum to remove bubbles, adding a foaming agent, mixing uniformly again, adjusting the pH to 6.9, homogenizing and emulsifying to obtain the liquid toothpaste.
Example III
A mild anticarious children liquid toothpaste comprises the following components in percentage by weight: 0.5% of cinnamic acid modified chitosan nano particles, 1.2% of essence, 0.3% of lactobacillus paracasei ADP-1, 2.0% of calcium glycerophosphate, 0.2% of casein phosphopeptide, 0.1% of compound amino acid composition, 0.2% of xylitol, 1.0% of cocamidopropyl betaine, 1.0% of laurylglucoside, 1.0% of sodium lauroyl glutamate, 0.2% of xanthan gum, 0.2% of cellulose gum, 0.1% of carbomer, 55% of sorbitol, 8% of polyethylene glycol, 15.0% of silicon dioxide, 0.1% of sucralose, 0.5% of sodium benzoate, 0.5% of coloring agent and the balance of deionized water; the compound amino acid composition comprises the following components in percentage by weight: 63.5% of water, 7% of lysine, 10% of arginine, 10% of glycine, 8% of histidine, 0.7% of 1, 2-hexanediol and 0.8% of p-hydroxyacetophenone.
The preparation method of the cinnamic acid modified chitosan nanoparticle comprises the following steps:
step 1: under the protection of argon, 2.0g/L H is added into 2.5g/L chitosan solution 2 O 2 Adding 8mg/L ascorbic acid into the solution, and adding cinnamic acid to react at 30 ℃ for 12 hours in an oscillating way; placing the reaction product into 14000Da dialysis bag, dialyzing, and lyophilizing to obtain cinnamic acid-chitosan graft copolymer, wherein chitosan solution and H 2 O 2 The volume ratio of the solution to the ascorbic acid is 2:1:2, the molar ratio of cinnamic acid to chitosan is 3:1;
step 2: dissolving cinnamic acid-chitosan graft copolymer in citric acid buffer solution, preparing CA-CTS solution with concentration of 3.5%, and regulating pH to 5 for use;
step 3: taking a pullulan sterilizing solution with the concentration of 2.0%, and carrying out centrifugal degassing treatment for later use; the rotational speed of the centrifugal degassing treatment is as follows: 4500r/min, 7min;
step 4: mixing the CA-CTS solution with the pullulan sterilizing solution after pH adjustment according to the mass ratio of 1:1, adding the compound vitamin into the obtained mixed solution, wherein the mass ratio of the mixed solution to the compound vitamin is 13:1, then rapidly stirring for 3 hours at 15 ℃, and carrying out atomization drying to obtain cinnamic acid modified chitosan nano particles; wherein the compound vitamin consists of vitamin D, vitamin K and vitamin C according to the mass ratio of 1:1:2.
A preparation method of mild anticarious children liquid toothpaste comprises the following steps:
step 1: preparing a composite amino acid composition, adding the amino acid components into deionized water according to a proportion, fully stirring, adding 1, 2-hexanediol and p-hydroxyacetophenone while stirring, and stirring until the amino acid components are completely dissolved;
step 2: preparing a first composition, swelling the thickener, mixing humectant, foaming agent, sodium benzoate and water according to weight percentage, stirring at 55deg.C, adding the thickener while stirring, stirring and dispersing uniformly until no lump exists, standing for 18 hr, and observing the solution to be uniform transparent thick liquid;
step 3: preparing a toothpaste composition, homogenizing, emulsifying and mixing a first composition, a composite amino acid composition, cinnamic acid modified chitosan nano particles, lactobacillus paracasei ADP-1 and an auxiliary agent according to a proportion;
step 4: adding the toothpaste composition into a paste making machine, adding silicon dioxide, stirring uniformly, simultaneously starting vacuum to remove bubbles, adding a foaming agent, mixing uniformly again, adjusting the pH to 7.1, homogenizing and emulsifying to obtain the liquid toothpaste.
Example IV
A mild anticarious children liquid toothpaste comprises the following components in percentage by weight: 1.0% of cinnamic acid modified chitosan nano particles, 0.5% of essence, 0.05% of lactobacillus paracasei ADP-1, 0.5% of sodium monofluorophosphate, 0.5% of calcium glycerophosphate, 0.05% of casein phosphopeptide, 0.05% of compound amino acid composition, 0.05% of xylitol, 1.0% of sodium lauryl glucose carboxylate, 1.0% of sodium methyl cocoyl taurate, 1.0% of cocamidopropyl betaine, 0.2% of xanthan gum, 0.2% of carrageenan, 0.1% of carbomer, 70% of sorbitol, 2% of polyethylene glycol, 8.0% of silicon dioxide, 0.25% of sucralose, 0.2% of sodium benzoate, 0.6% of colorant and the balance of deionized water; the compound amino acid composition comprises the following components in percentage by weight: 79% of water, 3% of lysine, 7% of arginine, 8% of glycine, 2% of histidine, 0.5% of 1, 2-hexanediol and 0.5% of p-hydroxyacetophenone.
The preparation method of the cinnamic acid modified chitosan nanoparticle comprises the following steps:
step 1: under the protection of argon, 1.2g/L H is added into 1.5g/L chitosan solution 2 O 2 Adding cinnamic acid into the solution and 6mg/L ascorbic acid, and oscillating at 32 ℃ for 11.8h; placing the reaction product into 14000Da dialysis bag, dialyzing, and lyophilizing to obtain cinnamic acid-chitosan graft copolymer, wherein chitosan solution and H 2 O 2 The volume ratio of the solution to the ascorbic acid is 4:2:2, the molar ratio of cinnamic acid to chitosan is 3:1;
step 2: dissolving cinnamic acid-chitosan graft copolymer in citric acid buffer solution, preparing CA-CTS solution with concentration of 4.5%, and regulating pH to 5 for use;
step 3: taking a pullulan sterilizing solution with the concentration of 1.8%, and carrying out centrifugal degassing treatment for later use; the rotational speed of the centrifugal degassing treatment is as follows: 4200r/min, 8min;
step 4: mixing the CA-CTS solution with the pullulan sterilizing solution after pH adjustment according to the mass ratio of 1:2, adding the compound vitamin into the obtained mixed solution, wherein the mass ratio of the mixed solution to the compound vitamin is 14:1, then rapidly stirring for 2.6 hours at 17 ℃, and carrying out atomization drying to obtain cinnamic acid modified chitosan nano particles; wherein the compound vitamin consists of vitamin D, vitamin K and vitamin C according to the mass ratio of 2:1:3.
A preparation method of mild anticarious children liquid toothpaste comprises the following steps:
step 1: preparing a composite amino acid composition, adding the amino acid components into deionized water according to a proportion, fully stirring, adding 1, 2-hexanediol and p-hydroxyacetophenone while stirring, and stirring until the amino acid components are completely dissolved;
step 2: preparing a first composition, swelling the thickener, mixing humectant, foaming agent, sodium benzoate and water according to weight percentage, stirring at 48 ℃, adding the thickener while stirring, stirring and dispersing uniformly until no lump exists, standing for 15 hours, and observing that the solution is uniform transparent thick liquid;
step 3: preparing a toothpaste composition, homogenizing, emulsifying and mixing a first composition, a composite amino acid composition, cinnamic acid modified chitosan nano particles, lactobacillus paracasei ADP-1 and an auxiliary agent according to a proportion;
step 4: adding the toothpaste composition into a paste making machine, adding silicon dioxide, stirring uniformly, simultaneously starting vacuum to remove bubbles, adding a foaming agent, mixing uniformly again, adjusting the pH to 6.8, homogenizing and emulsifying to obtain the liquid toothpaste.
Example five
A mild anticarious children liquid toothpaste comprises the following components in percentage by weight: 1.8% of cinnamic acid modified chitosan nano particles, 0.3% of essence, 0.08% of lactobacillus paracasei ADP-1, 0.7% of sodium monofluorophosphate, 0.45% of calcium glycerophosphate, 0.8% of casein phosphopeptide, 0.06% of compound amino acid composition, 0.15% of xylitol, 1.5% of sodium lauryl glucose carboxylate, 0.5% of lauryl glucoside, 0.5% of sodium methyl cocoyl taurate, 0.1% of cellulose gum, 0.1% of carrageenan, 0.3% of carbomer, 55% of sorbitol, 10% of polyethylene glycol, 8.5% of silicon dioxide, 0.2% of sucralose, 0.25% of sodium benzoate, 0.3% of colorant and the balance of deionized water; the compound amino acid composition comprises the following components in percentage by weight: 59% of water, 10% of lysine, 10% of arginine, 10% of glycine, 10% of histidine, 0.6% of 1, 2-hexanediol and 0.4% of p-hydroxyacetophenone.
The preparation method of the cinnamic acid modified chitosan nanoparticle is the same as that of the example 1.
The preparation method of the mild anticarious children liquid toothpaste is the same as that of the example 1, and the components are replaced correspondingly.
Example six
A mild anticarious children liquid toothpaste comprises the following components in percentage by weight: 0.5% of cinnamic acid modified chitosan nano particles, 0.3% of essence, 1.2% of lactobacillus paracasei ADP-1.2% of sodium monofluorophosphate, 0.8% of calcium glycerophosphate, 0.5% of casein phosphopeptide, 0.1% of compound amino acid composition, 0.1% of xylitol, 2.0% of sodium lauryl glucose carboxylate, 0.5% of sodium methyl cocoyl taurate, 0.1% of xanthan gum, 0.2% of carrageenan, 0.2% of carbomer, 62% of sorbitol, 1.5% of polyethylene glycol, 9.2% of silicon dioxide, 0.15% of sucralose, 0.3% of sodium benzoate, 0.4% of colorant and the balance of deionized water; the compound amino acid composition comprises the following components in percentage by weight: 80% of water, 2% of lysine, 7% of arginine, 4% of glycine, 5% of histidine, 1, 2-hexanediol and 1% of p-hydroxyacetophenone.
The preparation method of the cinnamic acid modified chitosan nanoparticle is the same as that of the example 1.
The preparation method of the mild anticarious children liquid toothpaste is the same as that of the example 1, and the components are replaced correspondingly.
Example seven
A mild anticarious children liquid toothpaste comprises the following components in percentage by weight: 0.8% of cinnamic acid modified chitosan nano particles, 0.5% of essence, 0.07% of lactobacillus paracasei ADP-1, 0.7% of sodium monofluorophosphate, 1.1% of calcium glycerophosphate, 1.2% of casein phosphopeptide, 0.15% of compound amino acid composition, 0.15% of xylitol, 0.5% of cocamidopropyl betaine, 1% of sodium methyl cocoyl taurate, 1% of sodium lauroyl glutamate, 0.3% of xanthan gum, 0.2% of carrageenan, 35% of sorbitol, 25% of polyethylene glycol, 10% of silicon dioxide, 0.2% of sucralose, 0.35% of sodium benzoate, 0.2% of colorant and the balance of deionized water; the compound amino acid composition comprises the following components in percentage by weight: 75% of water, 3% of lysine, 6% of arginine, 6% of glycine, 9% of histidine, 0.5% of 1, 2-hexanediol and 0.5% of p-hydroxyacetophenone.
The preparation method of the cinnamic acid modified chitosan nanoparticle is the same as that of the example 1.
The preparation method of the mild anticarious children liquid toothpaste is the same as that of the example 1, and the components are replaced correspondingly.
Comparative example
A mild anticarious child fluid toothpaste differs from example 1 in that cinnamic acid modified chitosan nanoparticles are replaced with cinnamic acid, chitosan, pullulan, and vitamins D, K, and C.
The preparation method of the mild anticarious children liquid toothpaste is the same as that of the example 1, and the component content is correspondingly replaced.
In order to more clearly illustrate the invention, the invention has also been demonstrated by the following experiments:
1. and (3) bacteriostasis experiment detection:
1.1 test bacteria
Bacteria: streptococcus mutans CMCC32400, porphyromonas gingivalis ATCC 33277 and Lactobacillus paracasei ADP-1.
1.2 preparation of bacterial liquid
Phosphate buffer of 0.03mo1/L NaC 1.0g, KC 1.2g, na 2 HPO 4 2.30g、KH 2 P0 4 0.4g；
Sequentially dissolving the above reagents in 1000m1 deionized water, sterilizing at 115 ℃ for 15min under high pressure after complete dissolution, and storing in a refrigerator for standby;
taking a nutrient agar culture medium slant fresh culture (24 h) of test strain for 8-10 generations, washing lawn with 5m 1.03 mol/L phosphate buffer solution, uniformly suspending the strain, and diluting 1000 times with the phosphate buffer solution to obtain Streptococcus mutans CMCC32400 bacterial suspension, porphyromonas gingivalis ATCC 33277 bacterial suspension and Lactobacillus paracasei ADP-1 bacterial suspension respectively.
1.3 preparation of experimental group
(1) Test article: taking 1g of the toothpaste of the first embodiment, and completely dissolving the toothpaste with 100ml of deionized water for later use;
(2) Control: taking 1g of the toothpaste of the comparative example, and completely dissolving the toothpaste with 100ml of deionized water for later use;
(3) Blank reference: 100ml deionized water is ready for use
1.4 procedure
Taking 9 test tubes, equally dividing the test tubes into 3 groups, namely a test group, a control group and a blank control group, respectively, adding 5ml of test products into the 3 test tubes in the test group, respectively adding 5ml of control products into the 3 test tubes in the control group, and respectively adding 5ml of blank control products into the 3 test tubes in the blank control group; adding 10OUL Streptococcus mutans CMCC32400 bacterial suspension, 10OUL Porphyromonas gingivalis ATCC 33277 bacterial suspension and 10OUL Lactobacillus paracasei ADP-1 bacterial suspension into 3 test tubes of each group respectively, and uniformly mixing; and (3) placing 0.5mL of the sampling liquid into a test tube containing 5mL of phosphate buffer solution at 20min, 60min and 120min, fully and uniformly mixing, properly diluting, taking 3 dilutions of the sampling liquid, respectively sucking 0.5mL of the sampling liquid into a culture dish, pouring 15mL of nutrient agar cooled to 40 ℃ into the culture dish, rotating the culture dish to make the culture dish fully and uniformly, overturning a flat plate after agar solidification, and culturing at 30 ℃ for 48 hours to count viable bacteria colonies.
1.5 experimental results
Refer to table 1 and fig. 1 to 6.
The mild anticarious children liquid toothpaste has remarkable antibacterial effect, taking example 1 as an example, the antibacterial rate of the mild anticarious children liquid toothpaste on streptococcus mutans CMCC32400 and porphyromonas gingivalis ATCC 33277 is more than 99.93%, the bacterial activity of the lactobacillus paracasei ADP-1 is not influenced, the benign development of oral microecology is facilitated, the comparative group has good antibacterial effect, but the bactericidal property is too strong, the streptococcus mutans CMCC32400 and porphyromonas gingivalis ATCC 33277 are inhibited, meanwhile, the lactobacillus paracasei ADP-1 beneficial to the oral cavity is also inhibited, and the long-term development of tooth health is not facilitated, and the specific data are shown in the following table:
TABLE 1 antibacterial Property test data
2. Human body experiment detection:
2.1, the detector selects:
the volunteer test subjects 60 are selected, and the ages of men and women are respectively half, and the ages of men and women are distributed between 6 and 12 years, and the volunteer test subjects are divided into two groups, wherein the teeth of the first group of volunteers have obvious decayed teeth, and the teeth of the second group of volunteers are healthy and have no decayed teeth.
2.2 test method:
two groups of volunteers were brushed with the toothpaste prepared in example one 3 months before and with the toothpaste prepared in comparative example three months after, and the dental health of the volunteers was observed and recorded for the first three months and the last three months.
2.3 experimental results:
the mild caries-preventing children liquid toothpaste of the invention is followed up, wherein the first group has 12 cases of slight caries, 18 cases of obvious caries, 27 cases of caries symptoms are relieved after 3 months of using the toothpaste of the first embodiment, 3 cases of caries are not worsened, and the second group of volunteers do not find caries; the toothpaste of the comparative example was changed after 3 months, and the same was continued for 3 months, with 11 of the first group of volunteers having new plaque build-up on the surface of the teeth, 4 of the volunteers having caries enlargement, 3 of the second group of volunteers having new plaque build-up on the surface of the teeth.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (7)
1. A mild anticarious children liquid toothpaste, which is characterized in that: comprises the following components in percentage by weight: 0.5 to 2.0 percent of cinnamic acid modified chitosan nano particles, 0.01 to 2.0 percent of compound amino acid composition, 0.01 to 2.0 percent of lactobacillus paracasei ADP-1, 1.0 to 3.0 percent of foaming agent, 0.1 to 0.5 percent of thickening agent, 50 to 70 percent of humectant, 8.0 to 15.0 percent of silicon dioxide, 0.2 to 0.5 percent of sodium benzoate and the balance of deionized water;
the preparation method of the cinnamic acid modified chitosan nanoparticle comprises the following steps:
step 1: under the protection of argon, H is added into chitosan solution 2 O 2 Adding cinnamic acid into the solution and ascorbic acid, and carrying out oscillation reaction for 10-12 h at the temperature of 30-35 ℃; putting the reaction product into a dialysis bag of 12000-14000 Da for dialysis in deionized water, and finally, freeze-drying to obtain the cinnamic acid-chitosan graft copolymer; wherein the concentration of the chitosan solution is 1.0-5.0 g/L, H 2 O 2 The concentration of the solution is 1.0-2.0 g/L, the concentration of the ascorbic acid is 2-10 mg/L, chitosan solution and H 2 O 2 The volume ratio of the solution to the ascorbic acid is 1-5: 1 to 3: 1-2, wherein the molar ratio of cinnamic acid to chitosan is 3:1;
step 2: dissolving cinnamic acid-chitosan graft copolymer in a citric acid buffer solution, preparing a CA-CTS solution with the concentration of 0.5-5%, and regulating the pH value to 5-5.9 for later use;
step 3: taking a pullulan sterilizing solution with the concentration of 0.5-2.0%, and carrying out centrifugal degassing treatment for later use; the rotational speed of the centrifugal degassing treatment is as follows: 2500-4500 r/min for 3-8 min;
step 4: mixing the CA-CTS solution with the pullulan sterilizing solution after pH adjustment according to the mass ratio of 1:1-8, adding the compound vitamin into the obtained mixed solution, then rapidly stirring for 1-3 h at 15-20 ℃, and carrying out atomization drying to obtain the cinnamic acid modified chitosan nano particles.
2. The mild anticariogenic child fluid dentifrice according to claim 1, wherein: the composition also comprises at least one auxiliary agent with the following weight percentage: 0.01 to 2.0 percent of casein phosphopeptide, 0.01 to 2.0 percent of calcium glycerophosphate, 0.1 to 2.0 percent of xylitol, 0.5 to 0.7 percent of sodium monofluorophosphate, 0.5 to 1.2 percent of essence, 0.1 to 0.3 percent of sweetener, 0.2 to 0.5 percent of preservative and 0.1 to 1.0 percent of colorant.
3. The mild anticariogenic child fluid dentifrice according to claim 1, wherein: the foaming agent is at least one of sodium lauryl glucose carboxylate, lauryl glucoside, sodium lauroyl glutamate, sodium methyl cocoyl taurate and cocamidopropyl betaine.
4. The mild anticariogenic child fluid dentifrice according to claim 1, wherein: the thickener is at least two of xanthan gum, carrageenan, cellulose gum and carbomer.
5. The mild anticariogenic child fluid dentifrice according to claim 1, wherein: the humectant is at least one of sorbitol, polyethylene glycol, butanediol, propylene glycol and glycerol.
6. The mild anticariogenic child fluid dentifrice according to claim 1, wherein: the compound amino acid composition comprises the following components in percentage by weight: 50 to 80 percent of water, 1 to 10 percent of lysine, 1 to 10 percent of arginine, 1 to 10 percent of glycine, 1 to 10 percent of histidine, 0.5 to 1.0 percent of 1, 2-hexanediol and 0.2 to 1.0 percent of p-hydroxyacetophenone.
7. The mild anticariogenic child fluid dentifrice according to claim 1, wherein: in the step 4, the mass ratio of the mixed solution to the compound vitamin is 3-16:1, and the compound vitamin comprises at least one of the following components: vitamin D, vitamin K and vitamin C.
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| CN101665544A (en) * | 2009-10-10 | 2010-03-10 | 河南中医学院 | Chitosan grafting compound of cinnamic acid derivatives and application |
| CN106562923A (en) * | 2016-08-12 | 2017-04-19 | 广州悦创实业有限公司 | Oral care composition containing probiotics, and application of oral care composition to toothpaste |
| CN108324675A (en) * | 2018-04-04 | 2018-07-27 | 三椒口腔健康股份有限公司 | A kind of toothpaste and preparation method thereof containing Lactobacillus paracasei |
| CN111701014A (en) * | 2020-08-12 | 2020-09-25 | 好易康生物科技(广州)有限公司 | Toothpaste for children and preparation method thereof |
| CN114831923A (en) * | 2022-04-29 | 2022-08-02 | 苏州清馨健康科技有限公司 | Double-beneficial balanced toothpaste and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US11564878B2 (en) * | 2020-06-08 | 2023-01-31 | Paul O'Malley | Oral care product formulation |
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| CN101665544A (en) * | 2009-10-10 | 2010-03-10 | 河南中医学院 | Chitosan grafting compound of cinnamic acid derivatives and application |
| CN106562923A (en) * | 2016-08-12 | 2017-04-19 | 广州悦创实业有限公司 | Oral care composition containing probiotics, and application of oral care composition to toothpaste |
| CN108324675A (en) * | 2018-04-04 | 2018-07-27 | 三椒口腔健康股份有限公司 | A kind of toothpaste and preparation method thereof containing Lactobacillus paracasei |
| CN111701014A (en) * | 2020-08-12 | 2020-09-25 | 好易康生物科技(广州)有限公司 | Toothpaste for children and preparation method thereof |
| CN114831923A (en) * | 2022-04-29 | 2022-08-02 | 苏州清馨健康科技有限公司 | Double-beneficial balanced toothpaste and preparation method thereof |
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