CN113576942B

CN113576942B - Anti-sugar toothpaste and preparation method thereof

Info

Publication number: CN113576942B
Application number: CN202111088745.4A
Authority: CN
Inventors: 刘城
Original assignee: Meizhou Harmonious Biotechnology Co ltd
Current assignee: Liu Cheng
Priority date: 2021-09-16
Filing date: 2021-09-16
Publication date: 2023-01-24
Anticipated expiration: 2041-09-16
Also published as: CN113576942A

Abstract

The invention relates to the technical field of toothpaste, in particular to anti-sugar toothpaste and a preparation method thereof, wherein the anti-sugar toothpaste comprises the following components: 15-30% of silicon dioxide, 10-20% of glycerol, 10-20% of sorbitol, 5-10% of polypropylene glycol, 0.1-0.5% of cocamidopropyl betaine, 2-8% of aluminum hydroxide, 0.5-1% of collagen, 3-5% of orange powder, 0.5-1% of rice hull ash, 1-2% of calcium carbonate, 0.05-0.1% of bezoar, 0.05-0.1% of baicalein, 0.1-0.5% of chlorogenic acid, 0.1-0.5% of eucalyptus oil, 0.05-0.1% of nicotinamide, 5-10% of an enzyme preparation, 1-5% of active polypeptide liquid, 0.01-0.5% of an emulsion stabilizer and the balance of deionized water. The toothpaste contains enzyme preparation, which can decompose saccharide in oral cavity, reduce saccharide content in oral cavity, and establish good oral cavity environment.

Description

Anti-sugar toothpaste and preparation method thereof

Technical Field

The invention relates to the technical field of toothpaste, in particular to anti-sugar toothpaste and a preparation method thereof.

Background

Oral cavity problems such as gum discomfort, periodontitis, tooth yellowing, cavity odor and the like are mostly caused by incomplete oral cavity cleaning and increase of harmful bacteria in the oral cavity, and saccharides are main nutrient substances for propagation and growth of the bacteria, so that the removal of saccharides in the cavity is the main purpose of cleaning the cavity.

At present, toothpaste in the market mainly utilizes active ingredients in the toothpaste to sterilize and inhibit bacteria so as to achieve the problem of cavity repair, for example, if triclosan copolymer, chlorhexidine and other chemical reagents are added, triclosan can inhibit dental plaque and gingivitis, and the triclosan copolymer has long retention time in the oral cavity and good antibacterial effect; chlorhexidine has excellent bactericidal effect, but has large irritation to oral mucosa, is easy to cause mucosa injury, and is easy to cause other oral problems after long-term use.

Disclosure of Invention

The invention aims to provide the anti-sugar toothpaste, which contains the enzyme preparation, and during the tooth brushing process, the biological enzyme in the enzyme preparation decomposes the saccharides remained in the oral cavity, reduces the content of the saccharides in the oral cavity, especially on the teeth, reduces the breeding of bacteria and establishes a good oral environment.

The invention also aims to provide a preparation method of the anti-sugar toothpaste, which can ensure the activity of the enzyme preparation, avoid the enzyme preparation from cracking and prolong the shelf life of the toothpaste by mixing the raw materials step by step, grinding and mixing the raw materials in a toothpaste making machine and finally adding the enzyme preparation.

The technical problem to be solved by the invention is realized by adopting the following technical scheme.

In one aspect, the embodiment of the invention provides an anti-sugar toothpaste, which comprises the following components in parts by mass: 15-30% of silicon dioxide, 10-20% of glycerol, 10-20% of sorbitol, 5-10% of polypropylene glycol, 0.1-0.5% of cocamidopropyl betaine, 2-8% of aluminum hydroxide, 0.5-1% of yellow collagen, 3-5% of orange powder, 0.5-1% of rice hull ash, 1-2% of calcium carbonate, 0.05-0.1% of bezoar, 0.05-0.1% of baicalein, 0.1-0.5% of chlorogenic acid, 0.1-0.5% of eucalyptus oil, 0.05-0.1% of nicotinamide, 5-10% of an enzyme preparation, 1-5% of an active polypeptide solution, 0.01-0.5% of an emulsion stabilizer and the balance of deionized water.

In another aspect, an embodiment of the present invention provides a method for preparing an anti-sugar toothpaste, including the following steps: s1, preparing an enzyme preparation;

s2, mixing glycerol, sorbitol, polyethylene glycol, bezoar, baicalein, chlorogenic acid, eucalyptus oil and deionized water, and uniformly stirring;

s3, mixing silicon dioxide, cocamidopropyl betaine, collagen, orange powder, rice hull ash, calcium carbonate, nicotinamide and active polypeptide liquid, and uniformly stirring;

and S4, mixing the solution obtained in the step S2 and the solution obtained in the step S3, adding an emulsion stabilizer, grinding for 20-40min at a high speed in a three-in-one vacuum paste making machine, vacuum degassing, adding the enzyme preparation prepared in the step S1, and uniformly mixing to obtain the toothpaste body.

Compared with the prior art, the embodiment of the invention has at least the following advantages or beneficial effects:

1. in the invention, the enzyme preparation is added into the toothpaste component, during the process of tooth brushing, the enzyme preparation can decompose saccharide in the oral cavity, improve the cleanness of the oral cavity, cut off the nutrient substances of harmful bacteria along with the reduction of the saccharide, radically reduce the propagation of the bacteria and relieve the oral cavity problem; and the enzyme preparation has safe components and has small irritation to oral mucosa compared with chemical bactericides.

2. Eucalyptus oil is added into the toothpaste components, is a natural sterilizing and disinfecting substance, can reduce bacteria in the oral cavity, and has small irritation to the oral cavity; the addition of the granular rice husk ash and the calcium carbonate increases the friction force between the toothpaste and teeth in the tooth brushing process, improves the cleaning force and the cleaning effect, has excellent adsorption performance, can adsorb bacteria, food residues and other substances in the oral cavity in the tooth brushing process, and discharges the substances along with water, thereby improving the cleaning effect in tooth brushing.

3. In the components of the toothpaste, the baicalein, the chlorogenic acid and the active polypeptide solution are added, and the three have synergistic action to relieve inflammation in the oral cavity, clear away fire and relieve pain, and are matched with the nicotinamide, so that the toothpaste has the effects of sterilizing and diminishing inflammation, repairing oral mucosa, relieving gum swelling and pain, relieving oral ulcer pain and the like.

4. When the toothpaste is prepared, various raw materials are mixed step by step, and then the enzyme preparation is added for mixing, so that the activity of the enzyme preparation can be prevented from being damaged; and the active enzyme in the enzyme preparation does not contact with other components, thereby prolonging the shelf life of the toothpaste.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.

It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.

The embodiment of the invention provides an anti-sugar toothpaste which comprises the following components in parts by mass: 15-30% of silicon dioxide, 10-20% of glycerol, 10-20% of sorbitol, 5-10% of polypropylene glycol, 0.1-0.5% of cocamidopropyl betaine, 2-8% of aluminum hydroxide, 0.5-1% of collagen, 3-5% of orange powder, 0.5-1% of rice hull ash, 1-2% of calcium carbonate, 0.05-0.1% of bezoar, 0.05-0.1% of baicalein, 0.1-0.5% of chlorogenic acid, 0.1-0.5% of eucalyptus oil, 0.05-0.1% of nicotinamide, 5-10% of an enzyme preparation, 1-5% of active polypeptide liquid, 0.01-0.5% of an emulsion stabilizer and the balance of deionized water.

In some embodiments of the present invention, the anti-sugar toothpaste comprises the following components by mass fraction: 20% of silicon dioxide, 15% of glycerol, 15% of sorbitol, 8% of polypropylene glycol, 0.3% of cocamidopropyl betaine, 5% of aluminum hydroxide, 0.8% of xanthan gum, 4% of orange powder, 1% of rice hull ash, 1.5% of calcium carbonate, 0.1% of bezoar, 0.1% of baicalein, 0.3% of chlorogenic acid, 0.5% of eucalyptus oil, 0.05% of nicotinamide, 10% of an enzyme preparation, 3% of active polypeptide liquid, 0.1% of an emulsion stabilizer and the balance of deionized water. The components in the toothpaste are controlled within the proportion range, so that the shelf life of the toothpaste is long, and the cavity cleaning effect is good.

In some embodiments of the invention, the rice hull ash has a particle size of 100-200nm. The nano-scale rice hull ash is selected, has large specific surface area and good adsorption force, can adsorb foreign matters in the oral cavity when cleaning the oral cavity, improves the cleaning efficiency of the toothpaste, and can adsorb peculiar smell in the oral cavity to achieve the effect of refreshing breath.

In some embodiments of the invention, the calcium carbonate has a particle size of 300 to 400nm. The calcium carbonate with the particle size range can improve certain friction force, clean tartar on the surface of teeth and simultaneously can not damage enamel.

In some embodiments of the invention, the enzyme preparation is a double-layer microcapsule structure, chitosan, ethyl cellulose, carrageenan and agar are used as wall materials, and glucose oxidase, probiotics and sodium chloride are used as core materials. The double-layer microcapsule is wrapped by the core material of the glucose oxidase through the chitosan and the cellulose, so that the glucose oxidase is prevented from being directly contacted with other components in the toothpaste, the problem that the toothpaste is yellow due to the decomposition of the glucose oxidase in the storage process can be avoided, and the shelf life of the toothpaste is prolonged. In addition, carrageenan and agar are added into the double-layer microcapsule structure to form a hydrogel array, so that the hydrophilicity of the double-layer microcapsule is improved, and the compatibility of the enzyme preparation and other components of toothpaste is improved; the carrageenin and the agar are loaded on the surface of the double-layer microcapsule, and in the process of tooth brushing, the double-layer microcapsule is broken under the action of external force to release glucose oxidase and probiotics, decompose sugar in the oral cavity and reduce the sugar content in the oral cavity, thereby reducing the reproduction of bacteria radically, and relieving the yellowing of teeth and brightening the teeth after long-term use.

In some embodiments of the invention, the enzyme preparation comprises the following components in parts by mass: 20-30% of glucose oxidase, 20-30% of probiotics, 10-20% of chitosan, 10-20% of ethyl cellulose, 1-5% of sodium chloride, 5-10% of carrageenan and 5-10% of agar.

In some embodiments of the invention, the enzyme preparation comprises the following components in parts by mass: 25% of glucose oxidase, 25% of probiotics, 15% of chitosan, 15% of ethyl cellulose, 3% of sodium chloride, 7% of carrageenan and 10% of agar. The enzyme preparation with the double-layer microcapsule structure prepared according to the proportion has high activity of glucose oxidase, probiotics enter a dormant state under the action of 3% sodium chloride, the activity of the probiotics is maintained, and the probiotics and the glucose oxidase act together to provide the effect of decomposing sugar of the enzyme preparation.

In some embodiments of the present invention, the active polypeptide solution comprises the following components by mass fraction: 30-40% of carnosine, 30-40% of glutathione and the balance of deionized water. The carnosine and the glutathione have certain oxidation resistance and inflammation diminishing effects, and can relieve inflammation in the oral cavity by being matched with the bezoar, the baicalein and the chlorogenic acid, so that the analgesic effect is achieved, and the oral inflammation and the oral ulcer can be reduced after long-term use.

On the other hand, the embodiment of the invention provides a preparation method of the sugar-resistant toothpaste, which comprises the following steps: s1, preparing an enzyme preparation;

In some embodiments of the invention, the method of preparing the enzyme preparation comprises the steps of:

s11, adding an aqueous solution of glucose oxidase into a chitosan acetic acid solution, stirring for 1-2h until the mixture is uniformly mixed, and spray-drying a solution system to obtain powder A;

s12, dissolving carrageenan and agar into water, adding the powder A prepared in the step S11, uniformly stirring, standing for 30-60min, and performing spray drying to prepare a first microcapsule;

s13, dispersing ethyl cellulose into dichloromethane, adding probiotics, sodium chloride and the first microcapsule prepared in the step S12, uniformly stirring, adding petroleum ether, precipitating, filtering and drying to prepare powder B;

s14, dissolving carrageenin and agar into water, adding the powder B prepared in the step S13, uniformly stirring, standing for 30-60min, and performing spray drying to obtain the enzyme preparation.

Through the two times of wrapping, glucose oxidase is respectively used as a core material, a first shell is formed by wrapping chitosan and ethyl cellulose, probiotics are loaded on the shell, and a second shell is formed by wrapping chitosan and ethyl cellulose. The outer layer is wrapped with carrageenan and agar to form a hydrogel array, and the microcapsule structure can be broken under the action of external force to release glucose oxidase and probiotics, so that saccharides in the oral cavity can be cleaned.

The features and properties of the present invention are described in further detail below with reference to examples.

Examples

Each raw material was prepared according to the percentage in table 1. Wherein, in examples 1-3, the average particle size of the rice husk ash was 100nm and the average particle size of the calcium carbonate powder was 300nm; in examples 4 to 6, the rice husk ash had an average particle size of 200nm and the calcium carbonate powder had an average particle size of 300nm; in examples 7 to 8, the average particle size of rice husk ash was 200nm and the average particle size of calcium carbonate powder was 400nm; in examples 9 to 10, the rice husk ash had an average particle size of 150nm and the calcium carbonate powder had an average particle size of 350nm.

TABLE 1 EXAMPLES 1-10 toothpaste compositions in weight percent

The toothpastes of examples 1-10 were prepared according to the following procedure.

Examples 1 to 4:

s1, selecting a corresponding enzyme preparation;

and S4, mixing the solution obtained in the step S1 and the solution obtained in the step S2, adding an emulsion stabilizer, grinding for 40min at a high speed in a three-in-one vacuum paste making machine, vacuum degassing, adding the enzyme preparation obtained in the step S1, and uniformly mixing to obtain the toothpaste body.

Examples 5 to 6:

the difference from examples 1 to 4 is that in step S4, vacuum degassing was performed after high-speed grinding for 30min, and the remaining steps were the same as those of examples 1 to 4.

Examples 7 to 10:

the difference from examples 1 to 4 is that vacuum degassing was performed after high-speed grinding for 20min in step S4, and the remaining steps are the same as those of examples 1 to 4.

Specifically, the components and contents (mass percentages) of the enzyme preparations used in examples 1 to 10 are shown in Table 2, and the corresponding enzyme preparations were prepared according to the following procedures.

TABLE 2 Components and amounts of enzyme preparations of examples 1-10

The enzyme preparations of examples 1 to 4 were prepared by the following method:

s12, dissolving carrageenin and agar into water, adding the powder A prepared in the step S11, uniformly stirring, standing for 60min, and performing spray drying to prepare a first microcapsule;

s13, dispersing ethyl cellulose into dichloromethane, adding probiotics, sodium chloride and the first microcapsule prepared in the step S11, uniformly stirring, adding petroleum ether, precipitating, filtering and drying to prepare powder B;

s14, dissolving carrageenan and agar into water, adding the powder B prepared in the step S13, uniformly stirring, standing for 60min, and performing spray drying to obtain the enzyme preparation.

Examples 5 to 6:

the difference from the enzyme preparation steps of examples 1 to 4 is that, in step S12, the time for standing is 30min; in step S14, the time for standing was 40min, and the rest was the same as in examples 1 to 4.

The enzyme preparation production steps of examples 7 to 10 were different in that, in step S12, the time for standing was 40min; in step S14, the time for standing was 30min, and the rest was the same as in examples 1 to 4.

Specifically, the components and contents (mass percentages) of the active polypeptides used in examples 1 to 10 are shown in Table 3.

TABLE 3 Components and amounts of active polypeptide solutions of examples 1-10

Selecting carnosine and glutathione with corresponding contents, adding deionized water, and uniformly mixing.

Comparative example

Comparative example 1

The difference from example 1 is that in comparative example 1, the enzyme preparation in example 1 was not added, and ethyl cellulose of equal weight was used instead of the enzyme preparation in example 1, and the rest of the formulation and procedure were the same as in example 1.

Comparative example 2

The difference from example 1 is that in comparative example 2, glucose oxidase, probiotics and sodium chloride available in the market are directly added into the toothpaste, i.e. in step 4, glucose oxidase, probiotics and sodium chloride are directly added, and the rest steps and the proportion are the same as those of example 1.

Comparative example 3

The difference from example 1 is that in comparative example 3, the preparation method of the enzyme preparation is different, specifically in step S14, carrageenan and agar are not added, and chitosan of equal weight is used instead of carrageenan and agar in example 1; the rest of the formulation and procedure were the same as in example 1.

Examples of the experiments

1. Measurement of sugar decomposition efficiency

Respectively preparing 10% glucose solution by mass percent, and placing the glucose solution in a container for later use; 3g of the toothpastes of examples 1 to 10 and comparative examples 1 to 3 were selected and placed on a toothbrush, and after the toothbrush loaded with the toothpastes was brushed back and forth on the container, i.e., the wall (below the liquid surface) for 5 minutes, the glucose content of the glucose solution in the container was measured immediately, and the results thereof are shown in Table 4. Wherein the decomposition rate = [ (initial concentration of glucose solution-concentration after decomposition)/initial concentration ] × 100%.

TABLE 4 glucose decomposition efficiency of the toothpastes of examples 1-10 and comparative examples 1-3

As can be seen from the above Table 4, the toothpastes of examples 1-10 have a decomposition efficiency of glucose of 50% or more, and can effectively decompose saccharides in the oral cavity when the toothpastes of the present invention are used for tooth brushing; in examples 1 to 10, an enzyme preparation having a double-layer microcapsule structure was added to release glucose oxidase and probiotics and decompose saccharides during tooth brushing. In comparative example 1, glucose oxidase was not added to the toothpaste, and the decomposition efficiency of glucose was 18%, and the decomposition efficiency was low, whereas in comparative example 2, glucose oxidase and probiotics were directly added, and the decomposition efficiency of glucose was 35, because glucose oxidase and probiotics were directly added to the toothpaste, and glucose oxidase directly contacted with other ingredients of the toothpaste, and the activity of glucose oxidase was reduced, and the decomposition efficiency of glucose was reduced. In comparative example 3, the enzyme preparation having a microcapsule structure was added, but carrageenan and agar were not added, and the enzyme preparation having a microcapsule structure was not easily broken during tooth brushing, and released less glucose oxidase, thereby having low glucose decomposition efficiency.

2. Toothpaste stability assay

The toothpastes of examples 1 to 10 and comparative examples 1 to 3 were extruded on a petri dish, and after being left in an oven at 25 c and an oven at 40 c, respectively, for 30min, the morphology of the toothpaste was observed, and the viscosity and pH of the toothpaste were measured, and the results thereof are shown in table 5.

TABLE 5 stability of examples 1-10 and comparative examples 1-3

As can be seen from Table 5, the toothpastes of examples 1-10 were slightly yellow after 30min of treatment at 40 ℃ because the glucose oxidase was decomposed, resulting in the toothpaste being yellow. The toothpastes of examples 1-10 were slightly yellow or normal, indicating that the enzyme preparation with double-layer microcapsule structure has good protective effect on glucose oxidase, and can prolong the effective period of glucose oxidase, i.e. prolong the shelf life of the toothpaste. In comparative example 2, glucose oxidase and probiotics were directly added to toothpaste, and the glucose oxidase was easily decomposed to cause yellowing of toothpaste, resulting in a short shelf life of glucose oxidase in toothpaste and a short shelf life of toothpaste.

3. Determination of antibacterial Properties of toothpastes

Randomly selecting 80 subjects, dividing into 8 groups, and using the toothpastes of examples 1-5 and comparative examples 1-3 respectively, brushing teeth once every morning and evening, using 2g of the toothpaste each time, and continuously using for 3 months; before, 1 month after, 2 months after and 3 months after the use of the toothpaste, the bacteria on the back of the tongue of the subject were collected, respectively, and then the collected samples were cultured in a blood agar medium at 37 ℃ under anaerobic conditions, and after 72 hours, the average bacterial colony forming unit was calculated, and the results are shown in table 6. Wherein the colony reduction rate = [ (initial colony unit-colony unit after use)/initial colony unit ] × 100%.

TABLE 6 results of clinical trials of toothpastes for examples 1-5 and comparative examples 1-3

As can be seen from the above Table 6, the toothpaste of examples 1-5 has excellent antibacterial property, the number of bacterial colonies in the oral cavity is reduced after 1 month of continuous use, and the bacterial colony reduction rate in the oral cavity reaches 71-82% after 3 months of continuous use, so that the number of bacteria in the oral cavity is effectively inhibited, the bacterial growth is reduced, and the effect of brightening and whitening teeth is achieved. In comparative examples 1-3, after continuous use for 3 months, the number of bacterial colonies is reduced, but the reduction rate is less, and the reduction rate is about 36-40%, which shows that the toothpaste of the invention has good effect on decomposing sugar in the oral cavity, inhibits the growth of bacteria radically, improves the microenvironment of the oral cavity and improves the oral cavity problem.

The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims

1. The anti-sugar toothpaste is characterized by comprising the following components in parts by mass: 15-30% of silicon dioxide, 10-20% of glycerol, 10-20% of sorbitol, 5-10% of polypropylene glycol, 0.1-0.5% of cocamidopropyl betaine, 2-8% of aluminum hydroxide, 0.5-1% of yellow collagen, 3-5% of orange powder, 0.5-1% of rice hull ash, 1-2% of calcium carbonate, 0.05-0.1% of bezoar, 0.05-0.1% of baicalein, 0.1-0.5% of chlorogenic acid, 0.1-0.5% of eucalyptus oil, 0.05-0.1% of nicotinamide, 5-10% of an enzyme preparation, 1-5% of an active polypeptide solution, 0.01-0.5% of an emulsion stabilizer and the balance of deionized water;

the enzyme preparation is of a double-layer microcapsule structure, chitosan, ethyl cellulose, carrageenan and agar are taken as wall materials, and glucose oxidase, probiotics and sodium chloride are taken as core materials;

the enzyme preparation comprises the following components in parts by mass: 20-30% of glucose oxidase, 20-30% of probiotics, 10-20% of chitosan, 10-20% of ethyl cellulose, 1-5% of sodium chloride, 5-10% of carrageenan and 5-10% of agar;

the preparation method of the enzyme preparation comprises the following steps:

2. The anti-sugar toothpaste according to claim 1, which comprises the following components in parts by mass: 20% of silicon dioxide, 15% of glycerol, 15% of sorbitol, 8% of polypropylene glycol, 0.3% of cocamidopropyl betaine, 5% of aluminum hydroxide, 0.8% of xanthan gum, 4% of orange powder, 1% of rice hull ash, 1.5% of calcium carbonate, 0.1% of bezoar, 0.1% of baicalein, 0.3% of chlorogenic acid, 0.5% of eucalyptus oil, 0.05% of nicotinamide, 10% of an enzyme preparation, 3% of active polypeptide liquid, 0.1% of an emulsion stabilizer and the balance of deionized water.

3. The anti-sugar toothpaste according to claim 1, wherein the rice husk ash has a particle size of 100-200nm.

4. The sugar-resistant toothpaste according to claim 1, wherein the calcium carbonate has a particle size of 300-400nm.

5. The sugar-resistant toothpaste according to claim 1, wherein the enzyme preparation comprises the following components in parts by mass: 25% of glucose oxidase, 25% of probiotics, 15% of chitosan, 15% of ethyl cellulose, 3% of sodium chloride, 7% of carrageenan and 10% of agar.

6. The sugar-resistant toothpaste according to claim 1, wherein the active polypeptide liquid comprises the following components in parts by mass: 30-40% of carnosine and 30-40% of glutathione, and the balance of deionized water.

7. A process for preparing an anti-sugar toothpaste according to any one of claims 1 to 6 comprising the steps of:

s1, preparing an enzyme preparation;