CN107412131B

CN107412131B - Oral care liquid

Info

Publication number: CN107412131B
Application number: CN201710691704.1A
Authority: CN
Inventors: 覃青
Original assignee: Wuhan Meiyitang Dental Co ltd
Current assignee: Wuhan Meiyitang Dental Co ltd
Priority date: 2017-08-14
Filing date: 2017-08-14
Publication date: 2020-09-01
Anticipated expiration: 2037-08-14
Also published as: CN107412131A

Abstract

The invention discloses an oral care solution, which comprises the following raw materials: water, ethanol, glycerin monostearate, xylitol, sorbitol, plant extract, magnesium lithium silicate and a bacteriostatic agent. The oral care solution disclosed by the invention researches the influence of different types of surfactants on antibacterial performance and treatment efficacy, and screens out proper surfactants and dosage. The oral cavity cleaning agent is low in cost, safe and reliable, contains plant extracts with good taste acceptance and effective components for protecting teeth, is natural and pure in taste, has a remarkable effect of killing bacteria in the oral cavity, reducing internal heat and diminishing inflammation, is suitable for being used in the oral cavity in an untimely way and daily oral cavity care, can effectively clean the oral cavity and the teeth, relieves uncomfortable symptoms such as toothache, gingival bleeding, oral ulcer, gingivitis, periodontitis, sore throat and the like, and protects the health of the oral cavity.

Description

Oral care liquid

Technical Field

The invention relates to the technical field of oral care solution.

Background

Oral diseases are common frequently-occurring diseases caused by various pathogenic bacteria in the oral cavity, and directly affect the body health of people. People have also long been using various oral care products to prevent the occurrence of oral diseases. At present, the main products of daily chemical oral care can be divided into toothpaste, gargle and breath freshener, and the products mainly have the effects of cleaning teeth, whitening teeth, removing dental plaque, killing harmful bacteria in oral cavity, preventing decayed teeth, freshening breath and the like, and also have certain positive effects on treating oral diseases such as gingival inflammation and the like. Still other products such as food-based chewing gums, edible breath-cleansing tablets, and the like may also have more or less of the above-mentioned benefits.

Patent application No.: 201110087399.8 discloses an oral care composition that is a stable, flowable and swishable suspension comprising a suspending polymer. Optional additional components include abrasives, surfactants, flavorants, colorants, antiplaque agents, anticalculus agents, tooth desensitizers, fluoride ion sources, and sweeteners.

Patent application No.: 201380072086.2 provides an oral care composition suitable for imparting a temporary whitening effect to a tooth surface, the composition comprising: (a) a liquid continuous phase comprising water or a monohydric or polyhydric alcohol or a mixture thereof; (b) a particulate tooth surface whitening agent dispersed in the continuous phase; (c) a deposition aid for the particulate tooth surface whitening agent; (d) from 0.1 to 5 wt% (based on the total weight of the oral care composition) of one or more surfactants; characterised in that at least 50% by weight of the total surfactant (d) present in the composition is selected from the group consisting of nonionic surfactants, amphoteric or zwitterionic surfactants, calcium-tolerant anionic surfactants and mixtures thereof.

At present, the mouth wash sold in the market has the functions of cleaning and eliminating the peculiar smell in the oral cavity. Still other oral care solutions have plaque removal and bacterial killing effects in the oral cavity. However, both the mouth wash and the oral care solution have certain care effect on the oral cavity, but most users cannot tolerate the strange taste in the mouth washing process, and the mouth wash and the oral care solution are particularly difficult to adapt to children.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides an oral care solution. The oral care methods provided by the present invention can remove, for example, bacteria, food debris, biofilm, plaque, and/or may cause or induce various oral conditions.

The invention is realized by the following steps: an oral care solution comprises the following raw materials: water, ethanol, glycerin monostearate, xylitol, sorbitol, plant extract, magnesium lithium silicate and a bacteriostatic agent.

Further, the oral care solution is prepared from the following raw materials in parts by weight: 90-105 parts of water, 3-7 parts of ethanol, 0.1-0.5 part of surfactant, 0.1-0.5 part of xylitol, 1-3 parts of sorbitol, 2-8 parts of plant extract, 0.3-1.3 parts of lithium magnesium silicate and 0.1-0.5 part of bacteriostatic agent.

The surfactant is a nonionic surfactant or an anionic surfactant, the nonionic surfactant is one or a mixture of more of glyceryl monostearate, sucrose decanoate and polyoxyethylene hydrogenated castor oil, and the anionic surfactant is one or a mixture of more of sodium lauryl sulfoacetate and sodium lauryl sulfate.

Further, the surfactant is a nonionic surfactant.

Still further, the surfactant is glyceryl monostearate.

The plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of (1-3): (2-4): (4-6) mixing, crushing and sieving by a sieve of 10-100 meshes to obtain plant raw materials; the plant raw materials are mixed with 5-95% ethanol water solution according to the mass ratio of 1: (10-30) leaching at 23-27 deg.C for 20-30 hr, filtering, centrifuging, rotary evaporating for concentration, and vacuum freeze drying.

Further, the plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of (1-3): (2-4): (4-6) mixing, crushing and sieving by a sieve of 10-100 meshes to obtain plant raw materials; adjusting the pH value of 35-45% ethanol water solution to 11-13 by using 0.1-0.5mol/L sodium hydroxide water solution, and then using 35-45% ethanol water solution with the pH value of 11-13 to prepare the plant raw material according to the feed liquid mass ratio of 1: (10-30) leaching at the temperature of 23-27 ℃ for 20-30 hours, filtering with 200-mesh 400-mesh filter cloth, centrifuging the filtrate at 3000-5000 r/min for 10-20 minutes, taking the supernatant, performing rotary evaporation concentration, concentrating the supernatant to 5-20% of the original volume to obtain a concentrated solution, performing vacuum freeze drying on the concentrated solution to obtain the product, controlling the material thickness to be 5-10mm, setting the pre-freezing temperature to be-30 to-20 ℃, keeping the sample temperature for 1-3 hours after the sample temperature is reduced to the set temperature, setting the sublimation temperature to be 5-15 ℃, the analysis temperature to be 30-40 ℃, the vacuum degree to be 10-20pa, and the drying time to be 10-16 hours.

Further, the plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of (1-3): (2-4): (4-6) mixing, crushing and sieving by a sieve of 10-100 meshes to obtain plant raw materials; adjusting the pH value of 35-45% ethanol water solution to 11-13 by using 0.1-0.5mol/L sodium hydroxide water solution, and then using 35-45% ethanol water solution with the pH value of 11-13 to prepare the plant raw material according to the feed liquid mass ratio of 1: (10-30) leaching for 20-30 hours at the temperature of 23-27 ℃ and the pressure of 400-.

The bacteriostatic agent is one or more of berberine, magnolol, and oxymatrine.

Further, the bacteriostatic agent is prepared from berberine and oxymatrine according to the mass ratio of (2-4): 1.

Enhancing oral health also brings benefits to systemic health, as oral tissue may be the route of systemic infection. Good oral health is associated with general health, including cardiovascular health. The oral care solutions of the present invention are useful for treating oral conditions in the mouth, and for cleaning the oral cavity and providing improved methods of enhancing oral health. The invention provides an oral care method, which is used for gargling by using the oral care solution daily, wherein the gargling frequency is 2-6 times per day.

The oral care solution disclosed by the invention researches the influence of different types of surfactants on antibacterial performance and treatment efficacy, and screens out proper surfactants and dosage. The oral cavity cleaning agent is low in cost, safe and reliable, contains plant extracts with good taste acceptance and effective components for protecting teeth, is natural and pure in taste, has a remarkable effect of killing bacteria in the oral cavity, reducing internal heat and diminishing inflammation, is suitable for being used in the oral cavity in an untimely way and daily oral cavity care, can effectively clean the oral cavity and the teeth, relieves uncomfortable symptoms such as toothache, gingival bleeding, oral ulcer, gingivitis, periodontitis, sore throat and the like, and protects the health of the oral cavity.

Detailed Description

And (3) testing the antibacterial performance:

the beef extract peptone agar culture medium for bacterial culture has the following specific formula: 3.0g of beef extract, 10g of peptone, 5.0g of sodium chloride, 20g of agar and 1000mL of water are heated to melt, and the pH value is adjusted to 7.4-7.6. Subpackaging, and sterilizing under high pressure and moist heat (121 deg.C, 20min) for use.

Strain: staphylococcus aureus (Staphylococcus aureus), Escherichia coli (Escherichia coli).

Transferring all tested strains to corresponding test tube slant culture medium, and repeating the inoculation of each strain. The bacteria are cultured in a biochemical incubator at 37 ℃ for 24h, and the mould is cultured at 28 ℃ for 48 h. 2 of each strain was used for the experiment, and the rest was refrigerated for further use.

Selecting each colony, inoculating to a plate, culturing bacteria for 24 hr, eluting with sterile normal saline, and making into 10-containing bacteria⁷CFU/mL of bacterial suspension. The preparation method comprises the following steps: respectively selecting a small amount of bacterial spores, washing with sterile normal saline, scattering glass beads, making into bacterial suspension, and adjusting the concentration of the bacterial suspension to 10⁷CFU/mL, spare.

And (3) carrying out dry heat sterilization on a circular blank filter paper sheet with the diameter of 6mm at 160 ℃, and storing the blank filter paper sheet for later use under the aseptic condition. 0.1mL of each activated experimental bacterial suspension with the bacterial liquid concentration adjusted is sucked by a sterile pipettor and added into a culture dish poured with the culture medium, and the bacterial suspension is uniformly coated by a self-made glass coater sterilized by dry heat. Then, the filter paper sheets are clamped by using sterile tweezers and placed on different bacteria-containing culture dishes, 10 mu L of oral care solution is absorbed on each filter paper sheet by using a sterile pipettor, and each bacteria is made into two dishes in parallel. The corresponding extraction solvent was then used as a negative control. Culturing the bacteria in a biochemical incubator at a constant temperature of 37 ℃ for 24h, measuring the diameter of a bacteriostatic circle by a cross method, and taking an average value.

In the examples, gallnut, Latin scientific name: rhus chinensis Mill, provided by Xiangguang medicinal materials Co., Ltd, Xiyao county, Yunnan, as a place of origin.

In the examples, the pomegranate rind is a dried pericarp of Punica granatum L. Supplied by Baichun pharmaceutical industries, Inc., Bozhou, the origin Shandong.

Clove, Latin scientific name: syzygiumaromaticum, a cloves available from baichu pharmaceutical limited, china, guangxi, a country of origin.

In the embodiment, the lithium magnesium silicate is magnesium lithium silicate gel of a model WSG-232 provided by Nanjing Weipu powder engineering research institute.

Examples glyceryl monostearate, CAS number: 31566-31-1.

Examples berberine, CAS number: 2086-83-1.

Examples oxymatrine, CAS number: 16837-52-8.

Examples 1 to 5

The oral care liquid comprises the following raw materials in parts by weight: 100 parts of deionized water, 5 parts of ethanol, 0.2 part of surfactant (the type of the surfactant is shown in table 1), 0.3 part of xylitol, 2 parts of sorbitol, 5 parts of plant extract, 0.8 part of lithium magnesium silicate and 0.12 part of berberine. Adding ethanol, surfactant, xylitol, sorbitol, plant extract, lithium magnesium silicate, and berberine into deionized water, and mixing to obtain oral care liquid.

The plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of 2: 3: 5, mixing, crushing and sieving by a 60-mesh sieve to obtain a plant raw material; using 40% ethanol water solution (namely ethanol water solution, wherein the volume fraction of ethanol is 40%) to prepare the plant raw material according to the mass ratio of 1: 20, leaching at the temperature of 25 ℃ for 24 hours, filtering by using 300-mesh filter cloth, centrifuging the filtrate at 4000 rpm for 15 minutes, taking the supernatant, carrying out rotary evaporation concentration, concentrating the supernatant to 10% of the original volume to obtain a concentrated solution, carrying out vacuum freeze drying on the concentrated solution to obtain the product, controlling the thickness of the material to be 6mm, setting the pre-freezing temperature to be-25 ℃, keeping the sample temperature for 2 hours after the sample temperature is reduced to the set temperature, setting the sublimation temperature to be 10 ℃, the resolution temperature to be 35 ℃, the vacuum degree to be 15pa, and drying for 12 hours.

Table 1: surfactant type and oral care solution antibacterial performance test result table

As shown in Table 1, the surfactant is glyceryl monostearate, and the oral care solution has optimal antibacterial performance.

Example 6

The oral care liquid comprises the following raw materials in parts by weight: 100 parts of deionized water, 5 parts of ethanol, 0.2 part of glycerin monostearate, 0.3 part of xylitol, 2 parts of sorbitol, 5 parts of plant extract, 0.8 part of lithium magnesium silicate and 0.12 part of berberine. Adding ethanol, glyceryl monostearate, xylitol, sorbitol, plant extract, magnesium lithium silicate, and berberine into deionized water, and mixing to obtain oral care liquid.

The plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of 2: 3: 5, mixing, crushing and sieving by a 60-mesh sieve to obtain a plant raw material; adjusting the pH of a 40% ethanol aqueous solution (namely the ethanol aqueous solution, wherein the volume fraction of ethanol is 40%) to 12 by using a 0.2mol/L sodium hydroxide aqueous solution, and then adjusting the pH of the plant raw material by using a pH 12 40% ethanol aqueous solution according to the mass ratio of the raw material liquid to the feed liquid of 1: 20, leaching at the temperature of 25 ℃ for 24 hours, filtering by using 300-mesh filter cloth, centrifuging the filtrate at 4000 rpm for 15 minutes, taking the supernatant, carrying out rotary evaporation concentration, concentrating the supernatant to 10% of the original volume to obtain a concentrated solution, carrying out vacuum freeze drying on the concentrated solution to obtain the product, controlling the thickness of the material to be 6mm, setting the pre-freezing temperature to be-25 ℃, keeping the sample temperature for 2 hours after the sample temperature is reduced to the set temperature, setting the sublimation temperature to be 10 ℃, the resolution temperature to be 35 ℃, the vacuum degree to be 15pa, and drying for 12 hours.

Example 7

The plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of 2: 3: 5, mixing, crushing and sieving by a 60-mesh sieve to obtain a plant raw material; using 40% ethanol water solution (namely ethanol water solution, wherein the volume fraction of ethanol is 40%) to prepare the plant raw material according to the mass ratio of 1: leaching 20 at 25 ℃ and 500MPa for 24 hours, filtering with 300-mesh filter cloth, centrifuging the filtrate at 4000 rpm for 15 minutes, taking the supernatant, performing rotary evaporation concentration, concentrating the supernatant to 10% of the original volume to obtain a concentrated solution, performing vacuum freeze drying on the concentrated solution to obtain the product, controlling the thickness of the material to be 6mm, setting the pre-freezing temperature to be-25 ℃, keeping the sample temperature for 2 hours after the sample temperature is reduced to the set temperature, setting the sublimation temperature to be 10 ℃, the analysis temperature to be 35 ℃, the vacuum degree to be 15pa, and drying for 12 hours.

Example 8

The plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of 2: 3: 5, mixing, crushing and sieving by a 60-mesh sieve to obtain a plant raw material; adjusting the pH of a 40% ethanol aqueous solution (namely the ethanol aqueous solution, wherein the volume fraction of ethanol is 40%) to 12 by using a 0.2mol/L sodium hydroxide aqueous solution, and then adjusting the pH of the plant raw material by using a pH 12 40% ethanol aqueous solution according to the mass ratio of the raw material liquid to the feed liquid of 1: leaching 20 at 25 ℃ and 500MPa for 24 hours, filtering with 300-mesh filter cloth, centrifuging the filtrate at 4000 rpm for 15 minutes, taking the supernatant, performing rotary evaporation concentration, concentrating the supernatant to 10% of the original volume to obtain a concentrated solution, performing vacuum freeze drying on the concentrated solution to obtain the product, controlling the thickness of the material to be 6mm, setting the pre-freezing temperature to be-25 ℃, keeping the sample temperature for 2 hours after the sample temperature is reduced to the set temperature, setting the sublimation temperature to be 10 ℃, the analysis temperature to be 35 ℃, the vacuum degree to be 15pa, and drying for 12 hours.

Example 9

The oral care liquid comprises the following raw materials in parts by weight: 100 parts of deionized water, 5 parts of ethanol, 0.2 part of glycerin monostearate, 0.3 part of xylitol, 2 parts of sorbitol, 5 parts of plant extract, 0.8 part of magnesium lithium silicate and 0.12 part of oxymatrine. Adding ethanol, glyceryl monostearate, xylitol, sorbitol, plant extract, magnesium lithium silicate, and oxymatrine into deionized water in sequence, and mixing to obtain oral care solution.

Example 10

The oral care liquid comprises the following raw materials in parts by weight: 100 parts of deionized water, 5 parts of ethanol, 0.2 part of glycerin monostearate, 0.3 part of xylitol, 2 parts of sorbitol, 5 parts of plant extract, 0.8 part of lithium magnesium silicate and 0.12 part of magnolol. Adding ethanol, glyceryl monostearate, xylitol, sorbitol, plant extract, magnesium lithium silicate, and magnolol into deionized water in sequence, and mixing to obtain oral care solution.

Example 11

The oral care liquid comprises the following raw materials in parts by weight: 100 parts of deionized water, 5 parts of ethanol, 0.2 part of glycerin monostearate, 0.3 part of xylitol, 2 parts of sorbitol, 5 parts of plant extract, 0.8 part of lithium magnesium silicate, 0.09 part of berberine and 0.03 part of oxymatrine. Adding ethanol, glyceryl monostearate, xylitol, sorbitol, plant extract, magnesium lithium silicate, berberine, and oxymatrine into deionized water in sequence, and mixing to obtain oral care solution. Oral care solution antibacterial performance test result: the diameter of the staphylococcus aureus inhibition zone is 19mm, and the diameter of the escherichia coli inhibition zone is 18 mm.

Test example 1

The oral care solutions prepared in examples 6-10 were tested for antibacterial performance, and the specific results are shown in table 2.

Table 2: EXAMPLES 6-10 oral Care solution antibacterial Performance test results Table

Test example 2

The oral care liquids prepared in example 1 and examples 6 to 11 were subjected to an oral ulcer treatment effect test.

Each group of objects: in 50 clinical observations (age 20-60 years), symptoms were: the oral mucosa has multiple ulcer surfaces with different sizes, and the ulcer surfaces have subjective pain, influence diet and have repeated attacks, wherein 25 men and 25 women have the ulcer surfaces.

The test subjects rinsed their mouths with 25g of oral care solution at 8 am, 12 am and 6 pm, respectively, for 2 weeks continuously, and the treatment effect was counted after 2 weeks.

The curative effect standard is as follows:

(1) and (3) healing: the symptoms disappear, and the ulcer surface is healed;

(2) the method has the following advantages: the ulcer is healed or obviously reduced, and the pain is obviously relieved or disappeared;

(3) and (4) invalidation: there was no significant symptom improvement before and after treatment.

Specific test data are shown in table 3. After comparison, statistical analysis is carried out, and the comparison result of each group shows that P is less than 0.05, and the difference has statistical significance.

Table 3: oral ulcer treatment effect test table

Experiments prove that the oral care solution can effectively improve the symptoms of oral ulcer, and the clinical effective rate is more than 94%. According to the invention, through researching the influence of different types of surfactants on the antibacterial performance and treatment efficacy of the oral care solution, the surfactant selected from glyceryl monostearate is the most ideal antibacterial performance of the oral care solution. The oral cavity cleaning agent is low in cost, safe and reliable, contains plant extracts with good taste acceptance and effective components for protecting teeth, is natural and pure in taste, has a remarkable effect of killing bacteria in the oral cavity, reducing internal heat and diminishing inflammation, is suitable for being used in the oral cavity in an untimely way and daily oral cavity care, can effectively clean the oral cavity and the teeth, relieves uncomfortable symptoms such as toothache, gingival bleeding, oral ulcer, gingivitis, periodontitis, sore throat and the like, and protects the health of the oral cavity.

Claims

1. An oral care solution is characterized by being prepared from the following raw materials in parts by weight: 90-105 parts of water, 3-7 parts of ethanol, 0.1-0.5 part of surfactant, 0.1-0.5 part of xylitol, 1-3 parts of sorbitol, 2-8 parts of plant extract, 0.3-1.3 parts of lithium magnesium silicate and 0.1-0.5 part of bacteriostatic agent;

the bacteriostatic agent is prepared from berberine and oxymatrine according to the mass ratio of (2-4): 1, preparing a composition;

the plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of (1-3): (2-4): (4-6) mixing, crushing and sieving by a sieve of 10-100 meshes to obtain plant raw materials; adjusting the pH value of 35-45% ethanol water solution to 11-13 by using 0.1-0.5mol/L sodium hydroxide water solution, and then using 35-45% ethanol water solution with the pH value of 11-13 to prepare the plant raw material according to the feed liquid mass ratio of 1: (10-30) leaching for 20-30 hours at the temperature of 23-27 ℃ and the pressure of 400-.

2. The oral care solution of claim 1, wherein: the surfactant is a nonionic surfactant or an anionic surfactant, the nonionic surfactant is one or a mixture of more of glyceryl monostearate, sucrose decanoate and polyoxyethylene hydrogenated castor oil, and the anionic surfactant is one or a mixture of more of sodium lauryl sulfoacetate and sodium lauryl sulfate.

3. The oral care solution of claim 1, wherein: the surfactant is a nonionic surfactant.

4. The oral care solution of claim 1, wherein: the surfactant is glyceryl monostearate.

5. An oral care solution is characterized by being prepared from the following raw materials in parts by weight: 100 parts of deionized water, 5 parts of ethanol, 0.2 part of glycerin monostearate, 0.3 part of xylitol, 2 parts of sorbitol, 5 parts of plant extract, 0.8 part of lithium magnesium silicate, 0.09 part of berberine and 0.03 part of oxymatrine; sequentially adding ethanol, glyceryl monostearate, xylitol, sorbitol, plant extract, lithium magnesium silicate, berberine and oxymatrine into deionized water, and mixing to obtain oral care solution;

the plant extract is prepared by the following method: gallnut, pomegranate bark and clove in a mass ratio of 2: 3: 5, mixing, crushing and sieving by a 60-mesh sieve to obtain a plant raw material; adjusting the pH value of 40% ethanol water solution to 12 by using 0.2mol/L sodium hydroxide water solution, and then adjusting the pH value of the plant raw material by using the water solution of the 40% ethanol with the weight ratio of 1: leaching 20 at 25 ℃ and 500MPa for 24 hours, filtering with 300-mesh filter cloth, centrifuging the filtrate at 4000 rpm for 15 minutes, taking the supernatant, performing rotary evaporation concentration, concentrating the supernatant to 10% of the original volume to obtain a concentrated solution, performing vacuum freeze drying on the concentrated solution to obtain the product, controlling the thickness of the material to be 6mm, setting the pre-freezing temperature to be-25 ℃, keeping the sample temperature for 2 hours after the sample temperature is reduced to the set temperature, setting the sublimation temperature to be 10 ℃, the analysis temperature to be 35 ℃, the vacuum degree to be 15pa, and drying for 12 hours.