CN115025015B

CN115025015B - Antibacterial mouthwash and preparation method thereof

Info

Publication number: CN115025015B
Application number: CN202210587840.7A
Authority: CN
Inventors: 吴岗; 周海林; 郭秀玲; 姜媛媛
Original assignee: Shenzhen Anduofu Disinfection High Tech Co ltd
Current assignee: Shenzhen Anduofu Disinfection High Tech Co ltd
Priority date: 2022-05-27
Filing date: 2022-05-27
Publication date: 2024-06-11
Anticipated expiration: 2042-05-27
Also published as: CN115025015A

Abstract

The application discloses antibacterial mouthwash and a preparation method thereof, and belongs to the field of oral care. An antibacterial mouthwash is prepared from the following raw materials in percentage by weight: 0.25-1% of polyvinylpyrrolidone iodine, 0.5-2% of menthol, 0.01-0.1% of xylitol, 0.05-0.2% of surfactant, 1-5% of humectant, 0.1-1% of preservative, 0.05-0.2% of pH regulator and the balance of water. A method for preparing antibacterial mouthwash, comprising the following steps: adding polyvinylpyrrolidone iodine, menthol, xylitol and a humectant into water, stirring and mixing, then continuously adding a surfactant and a pH regulator, stirring and mixing, finally adding a preservative, and stirring and mixing to obtain the antibacterial mouthwash. The application has the advantages of keeping the comfort of the mouth wash in use and obtaining good sterilization effect.

Description

Antibacterial mouthwash and preparation method thereof

Technical Field

The application relates to the field of oral care, in particular to antibacterial mouthwash and a preparation method thereof.

Background

Mouthwashes are common oral care products other than toothpastes, tooth powders, and are mainly used for cleaning the oral cavity, inhibiting bacterial reproduction in the oral cavity, masking off-flavors in the oral cavity, and leaving a pleasant and fresh sensation in the oral cavity. With the continuous importance of people on personal images and social etiquette, the market demand of mouthwash is increasing, and the function and quality requirements of mouthwash are also increasing.

The main components of the mouthwash comprise functional auxiliary agents, essence, humectant, surfactant, preservative, solvent and the like, wherein the functional auxiliary agents can be antibacterial agents, anticaries agents, gingivitis-preventing compounds, anti-inflammatory agents and the like so as to realize the functions of sterilizing, diminishing inflammation and resisting infection of the mouthwash, the surfactant can realize the function of cleaning the oral cavity, and the essence can realize the function of covering bad breath and other peculiar smell of the mouthwash, so that the mouthwash has more comprehensive effect.

At present, common mouthwash in the market is generally added with cetylpyridinium chloride as a bacteriostatic agent, the cetylpyridinium chloride has the effects of bacteriostasis and disinfection, and the sterilization effect of the mouthwash is improved, however, the addition of cetylpyridinium chloride can damage the mucous membrane which keeps the oral cavity moist and cause stinging sensation, so that the application and popularization of the mouthwash are limited.

Disclosure of Invention

In order to keep the comfort of the mouthwash in use and obtain a good sterilization effect, the application provides an antibacterial mouthwash and a preparation method thereof.

In a first aspect, the application provides an antibacterial mouthwash which adopts the following technical scheme:

an antibacterial mouthwash is prepared from the following raw materials in percentage by weight:

0.25 to 1 percent of polyvinylpyrrolidone iodine;

menthol 0.5-2%;

Xylitol 0.01-0.1%;

0.05 to 0.2 percent of surfactant;

1-5% of humectant;

0.1 to 1 percent of preservative;

0.05 to 0.2 percent of pH regulator;

0 to 0.6 percent of antibacterial synergist;

0 to 0.5 percent of other additives;

The balance of water.

By adopting the technical scheme, the application takes the polyvinylpyrrolidone iodine as a bacteriostatic agent, and the polyvinylpyrrolidone iodine belongs to a broad-spectrum bactericidal medicament, so that pathogenic microorganisms such as bacteria, viruses and fungi are effectively killed, the low toxicity is realized, and the oral mucosa is not stimulated, so that the comfort of the mouthwash in use is maintained, and a good bactericidal effect is obtained.

According to the application, menthol and xylitol are added into the mouthwash, so that the menthol can clean the oral cavity, reduce gum sensitivity, the xylitol can prevent dental caries, has a remarkable antibacterial effect, can inhibit bacteria from being adsorbed on the surface of teeth to form dental plaque, and the menthol and xylitol act together with polyvinylpyrrolidone iodine, so that the sterilization and antibacterial performance of the mouthwash can be greatly improved.

Optionally, the antibacterial synergist comprises snow tea extract, hydroxypropyl chitosan and ethanol, wherein the weight ratio of polyvinylpyrrolidone iodine to the snow tea extract to the hydroxypropyl chitosan to the ethanol is 1 (0.45-0.63), 0.20-0.32 and 1.2-1.5.

By adopting the technical scheme, the snow tea extract contains substances with good antibacterial activity such as the snow tea extract and the depsipelas, so that bacteria in the oral cavity can be effectively reduced, the snow tea extract and the hydroxypropyl chitosan are matched in a synergistic way, the peculiar smell in the oral cavity can be further removed, the breath is kept fresh for a long time, the irritation of the snow tea extract to the oral mucosa is small, and the use comfort is improved.

Optionally, the antibacterial synergist comprises ethyl palmitate and ethanol, wherein the weight ratio of the xylitol to the ethyl palmitate to the ethanol is 1 (1.2-1.6) to 2-3.

By adopting the technical scheme, the ethyl palmitate can help to disperse and stabilize xylitol, so that the inhibition effect on dental plaque diffusion is improved, and teeth are kept clean.

Optionally, the surfactant is sodium methyl cocoyl taurate.

Through adopting above-mentioned technical scheme, methyl cocoyl taurine sodium belongs to amino acid formula surfactant, has good clean function, helps cleaing away the food residue between the teeth, and is little to the pungency of oral mucosa moreover, and the use experience is good.

Optionally, the preservative is methylparaben.

By adopting the technical scheme, the addition of the methylparaben can reduce the putrefaction of the mouthwash and play a role in long-acting bacteriostasis.

Optionally, the pH adjuster is citric acid.

By adopting the technical scheme, the citric acid can adjust the pH balance in the oral cavity, and is helpful for removing the fishy smell in the oral cavity.

Optionally, the humectant is sorbitol.

Optionally, the other additives include flavoring essence and sweetener.

By adopting the technical scheme, the essence and the sweetener can improve the mouth feel of the mouthwash, and further improve the comfort in use.

Optionally, the sweetener is stevioside.

Optionally, the essence is lemon essence.

In a second aspect, the preparation method of the antibacterial mouthwash provided by the application adopts the following technical scheme:

a method for preparing antibacterial mouthwash, comprising the following steps:

adding polyvinylpyrrolidone iodine, menthol, xylitol and a humectant into water, stirring and mixing, then continuously adding a surfactant and a pH regulator, stirring and mixing, finally adding a preservative, and stirring and mixing to obtain the antibacterial mouthwash.

By adopting the technical scheme, the addition sequence of the raw materials is controlled, so that the raw materials are fully dispersed in water, and the stable mouthwash with good functional effect is obtained.

Optionally, before adding the polyvinylpyrrolidone iodine, menthol, xylitol and humectant into water, adding the antibacterial synergist into the water, and stirring and mixing; the antibacterial synergist comprises a snow tea extract, hydroxypropyl chitosan and ethanol, wherein the weight ratio of polyvinylpyrrolidone iodine to the snow tea extract to the hydroxypropyl chitosan is 1 (0.45-0.63) (0.2-0.32) (1.2-1.5).

By adopting the technical scheme, before the polyvinylpyrrolidone iodine, menthol, xylitol and humectant are added into water, the snow tea extract and the hydroxypropyl chitosan are fully mixed and dispersed, so that the synergistic effect of the snow tea extract and the hydroxypropyl chitosan is brought into play, and the oral cavity peculiar smell is reduced for a long time.

Optionally, before adding the polyvinylpyrrolidone iodine, menthol, xylitol and humectant into water, adding the antibacterial synergist into the water, and stirring and mixing; the antibacterial synergist comprises ethyl palmitate and ethanol, wherein the weight ratio of the xylitol to the ethyl palmitate to the ethanol is 1 (1.2-1.6) to 2-3.

Optionally, the snow tea is dried, chopped, added into ethanol for ultrasonic extraction, and then filtered, and the filtrate is concentrated to obtain the snow tea extract.

Alternatively, the ultrasonic leaching time is 0.5-1 h, the ultrasonic frequency is 50-70 KHz, preferably the ultrasonic leaching time is 1h, and the ultrasonic frequency is 70KHz.

By adopting the technical scheme, most of the snow tea extract is insoluble in water, so that the active antibacterial substances in the snow tea can be extracted by extracting the snow tea with ethanol.

In summary, the application has the following beneficial effects:

1. The application takes the polyvinylpyrrolidone iodine as a bacteriostatic agent, and the polyvinylpyrrolidone iodine belongs to a broad-spectrum bactericidal medicament, effectively kills pathogenic microorganisms such as bacteria, viruses and fungi, has low toxicity and no irritation to oral mucosa, thereby keeping the comfort of the mouthwash in use and obtaining good bactericidal effect.

According to the application, menthol and xylitol are added into the mouthwash, so that the menthol can clean the oral cavity, reduce gum sensitivity, the xylitol can prevent dental caries, has a remarkable antibacterial effect, can inhibit bacteria from being adsorbed on the surface of teeth to form dental plaque, and the menthol and xylitol act together with polyvinylpyrrolidone iodine, so that the sterilization and antibacterial performance of the mouthwash can be greatly improved;

2. The snow tea extract and the hydroxypropyl chitosan are added, so that the antibacterial capacity is improved, and meanwhile, the peculiar smell of the oral cavity is further removed.

Detailed Description

The present application will be described in further detail with reference to examples and comparative examples.

Preparation example

The preparation method of the snow tea extract comprises the following steps:

Drying herba Saussureae Involueratae in oven at 65deg.C for 1.5 hr, taking out and cutting herba Saussureae Involueratae, adding herba Saussureae Involueratae fragments into ethanol, ultrasonic extracting for 1 hr at ultrasonic frequency of 70kHz, filtering, collecting filtrate, concentrating the filtrate by rotary evaporation, and vacuumizing to remove ethanol to obtain powdered herba Saussureae Involueratae extract.

Examples

Example 1

An antibacterial mouthwash is prepared from the following raw materials:

25g of polyvinylpyrrolidone iodine, 50g of menthol, 1g of xylitol, 5g of sodium methyl cocoyl taurate, 10g of methylparaben, 100g of sorbitol, 5g of citric acid and 9804g of water.

A method for preparing antibacterial mouthwash, comprising the following steps:

Adding polyvinylpyrrolidone iodine, menthol, xylitol and sorbitol into water, stirring and mixing for 5min, then continuously adding sodium methyl cocoyl taurate and citric acid, stirring and mixing for 5min, finally adding methylparaben, stirring and mixing for 2min, and obtaining the antibacterial mouthwash.

Example 2

An antibacterial mouthwash is prepared from the following raw materials:

100g of polyvinylpyrrolidone iodine, 200g of menthol, 10g of xylitol, 20g of sodium methyl cocoyl taurate, 100g of methylparaben, 500g of sorbitol, 20g of citric acid and 9050g of water.

A method for preparing antibacterial mouthwash, comprising the following steps:

Example 3

An antibacterial mouthwash is prepared from the following raw materials:

60g of polyvinylpyrrolidone iodine, 130g of menthol, 6g of xylitol, 14g of sodium methyl cocoyl taurate, 40g of methylparaben, 335g of sorbitol, 16g of citric acid and 9399g of water.

A method for preparing antibacterial mouthwash, comprising the following steps:

Example 4

This example differs from example 3 in the raw materials and method of preparation of the antibacterial mouthwash.

The raw materials of the antibacterial mouthwash also contain 57g of snow tea extract and 90g of ethanol, and the weight of the water is 9252g.

In the preparation method of the antibacterial mouthwash, before polyvinylpyrrolidone iodine, menthol, xylitol and sorbitol are added into water, the snow tea extract and ethanol are mixed, then added into water, and stirred and mixed for 10min.

Example 5

The raw materials of the antibacterial mouthwash also contain 57g of hydroxypropyl chitosan and 90g of ethanol, and the weight of the water is 9252g.

In the preparation method of the antibacterial mouthwash, before polyvinylpyrrolidone iodine, menthol, xylitol and sorbitol are added into water, hydroxypropyl chitosan and ethanol are mixed, then added into water, and stirred and mixed for 10min.

Example 6

The raw materials of the antibacterial mouthwash also contain antibacterial synergistic agent, wherein the antibacterial synergistic agent is formed by mixing the snowfield tea extract, the hydroxypropyl chitosan and the ethanol, and the weight of the water is changed into 9252g, wherein 37.8g of the snowfield tea extract, 19.2g of the hydroxypropyl chitosan and 90g of the ethanol.

In the preparation method of the antibacterial mouthwash, before polyvinylpyrrolidone iodine, menthol, xylitol and sorbitol are added into water, an antibacterial synergist is added into the water, and the mixture is stirred and mixed for 10min.

Example 7

The difference between this example and example 6 is that the raw material ratio of the antibacterial mouthwash is different.

27G of snow tea extract, 12g of hydroxypropyl chitosan, 72g of ethanol and 9288g of water in the antibacterial synergist of the embodiment.

Example 8

The raw materials of the antibacterial mouthwash also contain antibacterial synergists, wherein the antibacterial synergists are formed by mixing ethyl palmitate and ethanol, 7.2g of ethyl palmitate, 12g of ethanol and 9379.8g of water are changed into water.

Example 9

The difference between this example and example 8 is that the raw material ratio of the antibacterial mouthwash is different.

In the antibacterial synergist of this example, ethyl palmitate 9.6g, ethanol 18g, and water weight change to 9371.4g.

Example 10

This example differs from example 6 in the raw material composition and proportions of the antibacterial mouthwash.

The antibacterial synergist of the embodiment comprises a snowfield tea extract, hydroxypropyl chitosan, ethyl palmitate and ethanol, wherein the weight of the snowfield tea extract is 37.8g, the hydroxypropyl chitosan is 19.2g, the ethyl palmitate is 9.6g, the ethanol is 108g, and the water weight is 9224.4g.

Example 11

The raw materials of the antibacterial mouthwash also contain other additives, wherein the other additives consist of edible essence and sweetener, the edible essence is lemon essence, the lemon essence is 5g, the sweetener is stevioside, the stevioside is 5g, and the weight of the water is 9389g.

In the preparation method of the antibacterial mouthwash, after the preservative is added into water, other additives are added into water and stirred and mixed for 10min.

Example 12

This example differs from example 11 in the raw material composition and proportions of the antibacterial mouthwash.

In the other additives of this example, the weight of lemon essence 30g, stevioside 20g, and water was 9249g.

Comparative example

Comparative example 1

This comparative example differs from example 3 in the raw material composition and proportions of the antibacterial mouthwash.

Polyvinylpyrrolidone iodine is not added into the raw materials of the antibacterial mouthwash, and the weight of the water is 9459g.

Comparative example 2

Xylitol is not added into the raw materials of the antibacterial mouthwash, the weight of menthol becomes 20g, and the weight of water becomes 9515g.

Comparative example 3

This comparative example differs from example 6 in the raw material composition and proportions of the antibacterial mouthwash.

Polyvinylpyrrolidone iodine is not added into the raw materials of the antibacterial mouthwash, and the weight of the water is 9402g.

Effect detection test

Mouthwashes prepared in the various examples and comparative examples of the present application were tested.

According to WS/T650-2019 ' quantitative antibacterial and bacteriostatic effect evaluation method of suspension ' 5.2.1 ', antibacterial test is carried out, antibacterial rate is tested, test strains are escherichia coli and candida albicans, the action concentration of a mouthwash sample is stock solution, the action time is 1min, and the test results are shown in table 1.

According to WS/T650-2019 ' method for evaluating antibacterial and bacteriostatic effect ' 5.2.7 continuous antibacterial test ', a long-acting antibacterial test is carried out, the long-acting antibacterial rate is tested, the test strains are escherichia coli and candida albicans, a mouthwash sample is tested after being stored for 12 hours at room temperature, the working concentration of the mouthwash sample is stock solution, the working time is 1min, and the test results are shown in table 1.

Selecting 90 volunteers without oral diseases and between ages 25 and 35, randomly and averagely dividing the volunteers into 15 groups, respectively testing 15 types of mouthwashes prepared in the embodiment and the comparative example by each group of volunteers, firstly, carrying out gas-off on a sampling cup, then smelling the smell of the sampling cup, evaluating the degree of the peculiar smell in the oral cavity of the volunteers and scoring the smell, wherein the score ranges from 0 point to 10 point, the higher the score is the heavier the degree of the peculiar smell, then rinsing the mouth with mouthwash for 1min, then discharging the mouth wash, and after 8h, the volunteers are further carrying out gas-off on the sampling cup, evaluating the degree of the peculiar smell in the oral cavity of the volunteers and scoring the smell, calculating the difference between the score of the two times before and after calculation to be the peculiar smell removal value, taking the average value of the peculiar smell removal value of each group, and recording the result as shown in table 2.

Alternatively 15 volunteers aged 25 to 35 years without oral disease were given a score of 0 in plaque index (PLI) test by brushing teeth and the like on test day 1, and then were not subjected to brushing teeth for 2 days in normal operation, and were each rinsed with mouthwash for 1min each morning and evening, each volunteer was again subjected to plaque index test on teeth labeled 16 by day 3 using 15 mouthwashes prepared in examples and comparative examples of the present application, the score results being shown in table 2, wherein the score criteria were "0=plaque at gingival margin area, 1=plaque at gingival margin area but visible for visual inspection, plaque was visible at the tooth face with the probe tip, 2=moderate plaque was visible at gingival margin or adjacent face, 3=large amount of soft plaque was in gingival sulcus or gingival margin area and adjacent face", and the test results are shown in table 2.

Alternatively, 15 volunteers with no oral diseases and ages of 25-35 were selected, and each volunteer was rinsed for 1min with 15 mouthwashes prepared in examples and comparative examples according to the present application, and the mouthwashes were evaluated for tingling, tingling or no tingling, and the test results are shown in table 2.

TABLE 1

TABLE 2

	Oral malodour test	Plaque index	Evaluation of tingling sensation
				Example 1	4.2	1	No stinging feeling
Example 2	4.0	1	No stinging feeling
				Example 3	4.3	1	No stinging feeling
Example 4	3.8	1	No stinging feeling
				Example 5	4.5	1	No stinging feeling
Example 6	6.5	1	No stinging feeling
				Example 7	6.3	1	No stinging feeling
Example 8	5.0	0	No stinging feeling
				Example 9	5.3	0	No stinging feeling
Example 10	6.7	0	No stinging feeling
				Example 11	4.7	1	No stinging feeling
Example 12	4.2	1	No stinging feeling
				Comparative example 1	3.3	1	No stinging feeling
Comparative example 2	2.0	2	No stinging feeling
				Comparative example 3	4.7	1	No stinging feeling

From tables 1 and 2, it is understood that the addition of polyvinylpyrrolidone iodine in example 3 has good effects on antibacterial ability, oral odor removing ability and plaque inhibiting ability, and no stink feeling, as compared with comparative example 1.

Example 3 was compared with comparative example 2 in that menthol and xylitol were added in the range of (0.5% to 2%) and (0.01% to 0.1%) on the basis of adding povidone-iodine, thereby obtaining more excellent antibacterial ability and oral malodor removing ability.

Compared with the embodiment 3, the embodiment 4 adds the snow tea extract, so that the long-acting antibacterial capability of the mouthwash is improved; compared with example 3, the hydroxypropyl chitosan is added in example 5, and the mouthwash has no obvious effect improvement; compared with the embodiment 3, the embodiment 6-7 is added with the snow tea extract and the hydroxypropyl chitosan at the same time, the long-acting antibacterial capacity of the mouthwash is improved greatly, the oral cavity peculiar smell removing capacity is improved obviously, and the effect is more outstanding.

Compared with comparative example 3, example 3 contains polyvinylpyrrolidone iodine, snow tea extract and hydroxypropyl chitosan, and the mouthwash has good effects in terms of antibacterial ability and oral odor removing ability, which shows that the polyvinylpyrrolidone iodine, the snow tea extract and the hydroxypropyl chitosan can supplement each other to exert efficacy.

In examples 8-9, ethyl palmitate was added and the plaque inhibition ability of the mouthwash was significantly improved as compared to example 3.

Compared with example 3, the combined effect of example 10 added with ethyl palmitate, snow tea extract and hydroxypropyl chitosan is optimal.

The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.

Claims

1. An antibacterial mouthwash, characterized in that: the material consists of the following raw materials in percentage by weight:

0.6% of polyvinylpyrrolidone iodine;

Menthol 1.3%;

Xylitol 0.06%;

0.14% of a surfactant;

3.35% of humectant;

0.4% of preservative;

0.16% of pH regulator;

1.47% of antibacterial synergist;

92.52% of water;

The total amount of the raw materials is 10000g;

The antibacterial synergist comprises a snow tea extract, hydroxypropyl chitosan and ethanol, wherein the snow tea extract, the hydroxypropyl chitosan and the ethanol account for the antibacterial mouthwash in percentage by weight:

0.378% of snow tea extract;

Hydroxypropyl chitosan 0.192%;

Ethanol 0.9%;

The preparation method of the snow tea extract comprises the following steps: oven drying herba Saussureae Involueratae, cutting, adding ethanol, ultrasonic leaching, filtering, and concentrating the filtrate to obtain herba Saussureae Involueratae extract.

2. An antibacterial mouthwash, characterized in that: the material consists of the following raw materials in percentage by weight:

0.6% of polyvinylpyrrolidone iodine;

Menthol 1.3%;

Xylitol 0.06%;

0.14% of a surfactant;

3.35% of humectant;

0.4% of preservative;

0.16% of pH regulator;

1.11% of antibacterial synergist;

92.88% of water;

The total amount of the raw materials is 10000g;

0.27% of snow tea extract;

0.12% of hydroxypropyl chitosan;

Ethanol 0.72%;

3. An antibacterial mouthwash, characterized in that: the material consists of the following raw materials in percentage by weight:

0.25% -1% of polyvinylpyrrolidone iodine;

Menthol 0.5% -2%;

Xylitol 0.01% -0.1%;

0.05% -0.2% of a surfactant;

1% -5% of humectant;

0.1% -1% of preservative;

0.05% -0.2% of pH regulator;

0.192% -0.6% of antibacterial synergist;

0% -0.5% of other additives;

The balance of water;

The antibacterial synergist comprises ethyl palmitate and ethanol, wherein the weight ratio of xylitol to ethyl palmitate to ethanol is 1 (1.2-1.6): 2-3.

4. An antibacterial mouthwash, characterized in that: the material consists of the following raw materials in percentage by weight:

0.6% of polyvinylpyrrolidone iodine;

Menthol 1.3%;

Xylitol 0.06%;

0.14% of a surfactant;

3.35% of humectant;

0.4% of preservative;

0.16% of pH regulator;

a bacteriostatic synergist 1.746%;

Water 92.244%;

The total amount of the raw materials is 10000g;

The antibacterial synergist comprises a snow tea extract, hydroxypropyl chitosan, ethyl palmitate and ethanol, wherein the snow tea extract, the hydroxypropyl chitosan, the ethyl palmitate and the ethanol account for the antibacterial mouthwash in percentage by weight:

0.378% of snow tea extract;

Hydroxypropyl chitosan 0.192%;

Ethyl palmitate 0.096%;

ethanol 1.08%;

5. An antibacterial mouthwash according to any one of claims 1 to 4, wherein: the surfactant is sodium methyl cocoyl taurate.

6. An antibacterial mouthwash according to any one of claims 1 to 4, wherein: the preservative is methylparaben.

7. An antibacterial mouthwash according to any one of claims 1 to 4, wherein: the pH regulator is citric acid.

8. The preparation method of the antibacterial mouthwash is characterized by comprising the following steps of: an antibacterial mouthwash for use in the preparation of any one of claims 1 to 4, comprising the steps of:

adding polyvinylpyrrolidone iodine, menthol, xylitol and a humectant into water, stirring and mixing, then continuously adding a surfactant and a pH regulator, stirring and mixing, finally adding a preservative, and stirring and mixing to obtain the antibacterial mouthwash;

Before adding the polyvinylpyrrolidone iodine, menthol, xylitol and humectant into water, adding the antibacterial synergist into the water, and stirring and mixing.