CN110327232B

CN110327232B - Ilicis cortex mouthwash

Info

Publication number: CN110327232B
Application number: CN201910741640.0A
Authority: CN
Inventors: 张义淦; 吴序栎; 陈嘉敏
Original assignee: Baiyinxiang Biotechnology Co ltd
Current assignee: Baiyinxiang Biotechnology Co ltd
Priority date: 2019-08-12
Filing date: 2019-08-12
Publication date: 2021-02-26
Anticipated expiration: 2039-08-12
Also published as: CN110327232A

Abstract

The invention belongs to the technical field of mouthwash, and particularly relates to rotunda thumb gargle which is prepared by carrying out soda water extraction twice and then carrying out alcohol extraction on the rotunda thumb gargle raw materials, wherein the rotunda thumb gargle raw materials comprise citric acid, edible spice, xylitol, menthol, ethanol and soda water.

Description

Ilicis cortex mouthwash

Technical Field

The invention belongs to the technical field of mouthwash, and particularly relates to ovate leaf holly bark mouthwash.

Background

With the increasing importance of oral care, mouthwash having a cleaning, cosmetic and/or functional therapeutic effect is coming into the field of vision of people. The mouthwash is convenient to use, is one of the modes for cleaning oral health, can reduce bacteria and bacterial plaque causing halitosis, and improves the gum health.

Although the types of mouthwashes on the market are various, they can be roughly divided into two types, namely health-care mouthwashes and therapeutic mouthwashes. Wherein the health-care mouth wash is available in a supermarket and has the functions of refreshing breath and removing food residues. The therapeutic mouth wash for treating periodontal diseases and oral mucosa diseases can be bought only in hospitals or drug stores.

The mouth wash is an indispensable oral cavity cleaning sanitary product in daily life of people, and has the basic functions of cleaning teeth, refreshing breath and achieving the aim of keeping the oral cavity clean. The function of the existing mouthwash on the market is single, and some chemical components contained in the mouthwash can not be frequently used for a long time; in the department of oral hospital mucous membrane, the situation that the patient suffers from new diseases or the original disease worsens often appears, therefore, consumer's health care consciousness is constantly strengthened, has proposed more requirements to the mouthwash, has increased some auxiliary prevention oral diseases in addition to cleaning the teeth, has the function of nursing health care effect to the oral cavity, consequently, the product that has various functional types in domestic and foreign mouthwash becomes the market mainstream, because traditional chinese medicine plant active ingredient has the incomparable advantage of western medicines such as nature, safety, the functional type mouthwash with traditional chinese medicine active ingredient becomes the key point of current development in the market again. In recent years, with the development of the modernization technology of traditional Chinese medicines, the method for researching and utilizing the active ingredients of the traditional Chinese medicines is well developed, and good technical support is provided for assisting in preventing oral diseases by utilizing the active ingredients of the traditional Chinese medicines in mouthwash.

Most of oral products declared to have antibacterial and anti-inflammatory effects at present adopt chemical bactericides, such as triclosan, cetylpyridinium chloride and the like as effective components, but the safety of the oral products is always worried by consumers: triclosan is reported to react with chlorine in tap water to produce chloroform, which is a carcinogenic hazard. The above disadvantages prevent consumers from using the product to reduce oral inflammation.

The ovate leaf holly bark is bark or root bark of ilex rotunda of Aquifoliaceae, is a common Chinese herbal medicine in southern folk, and has the following main functions: clearing away heat and toxic material, promoting diuresis, eliminating swelling and relieving pain. Modern pharmacological research shows that the ovate leaf holly bark has various pharmacological activities of increasing coronary flow, reducing blood pressure, resisting myocardial anoxia and resisting tumors, and also has obvious effect on inhibiting oral pathogenic bacteria. The main chemical components of the ovateleaf holly bark are triterpenes, flavonoids, phenols and the like.

The existing Chinese patent application CN 109512740A discloses an oral composition containing a liquorice extract and an ovate leaf holly bark extract and application thereof, wherein the oral composition has the liquorice extract and the ovate leaf holly bark extract and has the antibacterial effect, but the breath freshening and anti-inflammation effects of the oral composition are still to be improved.

Disclosure of Invention

In order to overcome the technical problems, the invention provides the ovate leaf holly bark mouthwash, so that the mouthwash has the functions of refreshing breath, keeping the oral cavity clean, inhibiting bacteria and diminishing inflammation.

In order to achieve the above purpose, the technical scheme provided by the invention is as follows:

an ovate leaf holly bark mouthwash comprises the following raw materials:

ovateleaf holly bark, citric acid, edible spice, xylitol, menthol, ethanol and soda water.

Preferably, the raw materials further comprise: aloe extract, chamomile extract.

Preferably, the mouthwash comprises the following raw materials in parts by weight: 8-13 parts of ovateleaf holly bark, 1-3 parts of aloe extract, 1-3 parts of chamomile extract, 0.1-0.5 part of citric acid, 0.1-0.5 part of edible spice, 1-2 parts of xylitol, 0.5-2 parts of menthol, 1-3 parts of ethanol and 75-90 parts of soda water.

Preferably, the mouthwash comprises the following raw materials in parts by weight: 12-13 parts of ovateleaf holly bark, 1-2 parts of aloe extract, 1-2 parts of chamomile extract, 0.2-0.3 part of citric acid, 0.1-0.3 part of edible spice, 1-1.5 parts of xylitol, 1-2 parts of menthol and 2-3 parts of ethanol; 80-85 parts of soda water.

Preferably, the mouthwash comprises the following raw materials in parts by weight:

11 parts of ovateleaf holly bark, 1 part of aloe extract, 1 part of chamomile extract, 0.2 part of citric acid, 0.3 part of edible spice, 1.5 parts of xylitol, 1 part of menthol and 2 parts of ethanol; 82 parts of soda water.

Preferably, the preparation method of the aloe extract comprises the following steps: cleaning folium Aloe, peeling, grinding into slurry, removing cellulose, precipitating with ethanol, centrifuging, filtering, and freeze drying to obtain Aloe extract;

preferably, the preparation method of the chamomile extract comprises the following steps: adding water into flos Matricariae Chamomillae, heating under reflux, filtering, rotary steaming, precipitating with ethanol, filtering, rotary steaming, and drying to obtain flos Matricariae Chamomillae extract;

the invention also aims to provide a preparation method of the rotunda officinalis mouthwash, which comprises the following steps:

(1) pulverizing cortex Ilicis Rotundae, adding half amount of soda water, extracting, adding the rest soda water, and extracting to obtain water extractive solution and residue;

(2) soaking the residue in ethanol solution, heating and refluxing, concentrating under reduced pressure, drying to remove ethanol to obtain cortex Ilicis Rotundae ethanol extract;

(3) dissolving menthol in ethanol to obtain menthol solution;

(4) adding the alcohol extract into the water extract, sequentially adding the aloe extract, the chamomile extract, the citric acid, the edible flavor and the xylitol, uniformly mixing, and adding the alcohol solution of the menthol to obtain the Ilicis rotunda Rotundae mouth wash.

Preferably, in the step (1), the crushed meshes of the ovate leaf holly bark are 60-80 meshes;

preferably, in step (1), the extraction is carried out at 50-70 ℃ for 1-2 h; the continuous extraction is carried out at 75-80 ℃ for 20-30 min;

preferably, in the step (2), the volume of the ethanol is 3-4 times of that of the residue, and the concentration of the ethanol is 50-60%;

preferably, in the step (2), the heating reflux is carried out at 85-90 ℃ for 2-3 h;

preferably, in the step (2), the concentration under reduced pressure is carried out at 60-75 ℃ and-0.06-0.08 MPa;

preferably, in the step (2), the drying is performed in vacuum drying, and the temperature of the vacuum drying oven is set to 40-60 ℃.

Preferably, the preparation method of the rotunda officinalis mouthwash comprises the following steps:

(1) pulverizing cortex Ilicis Rotundae to 60-80 mesh, adding half of soda water, extracting at 50-70 deg.C for 1-2 hr, adding the rest soda water, heating to 75-80 deg.C, and extracting for 20-30min to obtain water extractive solution and residue;

(2) soaking the residue in 3-4 times volume of 50-60% ethanol solution for 1-2 hr, heating and refluxing at 85-90 deg.C for 2-3 hr, concentrating at 60-75 deg.C under-0.06-0.08 Mpa under reduced pressure, and drying to remove ethanol to obtain cortex Ilicis Rotundae ethanol extract;

(3) dissolving menthol in ethanol to obtain menthol solution;

Compared with the prior art, the invention has the technical advantages that:

(1) the rotunda officinalis mouthwash prepared by the invention has good breath freshening and anti-inflammation effects;

(2) the aloe extract, the chamomile extract, the citric acid, the xylitol, the menthol and the ovate leaf holly bark have good synergistic effect, and can well promote the breath freshening, bacteriostasis and anti-inflammation effects of the ovate leaf holly bark;

(3) the aloe extract or chamomile extract used in the present invention may be prepared according to the method mentioned in the present invention, or may be a commercially available aloe extract or chamomile extract.

(4) The invention adopts a mode of combining water extraction and alcohol extraction to extract the ovate leaf holly bark, and can better extract the effective components in the ovate leaf holly bark to make the ovate leaf holly bark play a role;

(5) the mouthwash of the invention is extracted by soda water twice, which is more beneficial to the extraction of effective components and leads the extraction of the effective components to be more complete;

(6) in the invention, ethanol is removed after alcohol extraction, and then the specified amount of ethanol in the raw materials is added in the menthol dissolution, so that the ethanol content in the prepared mouthwash can be ensured to be stabilized in a controllable low concentration range, and the mouthwash is convenient to adapt to different people;

(7) the mouthwash provided by the invention has the advantages of fewer raw materials and lower cost.

Detailed Description

Example 1

Preparation of aloe extract: cleaning 5.0kg of folium Aloe, peeling, grinding into pulp, removing cellulose, adding 95% ethanol, precipitating with ethanol until the ethanol content of the solution reaches 60%, centrifuging, filtering, and freeze drying to obtain Aloe extract;

preparation of chamomile extract: taking 5.0kg of chamomile flowers, adding 12 times of distilled water, heating, refluxing and extracting for 3 times, wherein each time is 1.5h, filtering, combining extracting solutions, carrying out rotary evaporation until 1mL of solution contains 1g of crude drug, adding 95% ethanol, carrying out alcohol precipitation until the alcohol content of the solution reaches 60%, standing for 48h, filtering, carrying out rotary evaporation, and drying at the constant temperature of 60 ℃ to obtain the chamomile extract.

The aloe extract or chamomile extract of the following examples were prepared according to the method of this example.

Example 2

In the embodiment, the mouthwash comprises the following raw materials in parts by weight:

The preparation method of the rotunda officinalis mouthwash comprises the following steps:

(1) pulverizing cortex Ilicis Rotundae to 70 mesh, adding half of soda water, extracting at 60 deg.C for 1.5 hr, adding the rest soda water, heating to 75 deg.C, and extracting for 25min to obtain water extractive solution and residue;

(2) soaking the residue in 55% ethanol solution 3 times the volume of the residue for 1.5 hr, heating under reflux at 85 deg.C for 2.5 hr, concentrating under reduced pressure at 70 deg.C and-0.07 Mpa, vacuum drying at 45 deg.C to remove ethanol to obtain cortex Ilicis Rotundae ethanol extract;

(3) dissolving menthol in ethanol to obtain menthol solution;

Example 3

8 parts of ovateleaf holly bark, 1 part of aloe extract, 1 part of chamomile extract, 0.1 part of citric acid, 0.1 part of edible spice, 1 part of xylitol, 0.5 part of menthol, 1 part of ethanol and 75 parts of soda water.

(1) pulverizing cortex Ilicis Rotundae to 60 mesh, adding half of soda water, extracting at 50 deg.C for 1 hr, adding the rest soda water, heating to 75 deg.C, and extracting for 20min to obtain water extractive solution and residue;

(2) soaking the residue in 50% ethanol solution 3 times the volume of the residue for 1 hr, heating and refluxing at 85 deg.C for 2 hr, concentrating under reduced pressure at 60 deg.C and-0.06 Mpa, setting the temperature of vacuum drying oven at 40 deg.C, and drying to remove ethanol to obtain cortex Ilicis Rotundae ethanol extract;

(3) dissolving menthol in ethanol to obtain menthol solution;

Example 4

13 parts of ovateleaf holly bark, 3 parts of aloe extract, 3 parts of chamomile extract, 0.5 part of citric acid, 0.5 part of edible spice, 2 parts of xylitol, 2 parts of menthol, 3 parts of ethanol and 90 parts of soda water.

(1) pulverizing cortex Ilicis Rotundae to 80 mesh, adding half of soda water, extracting at 70 deg.C for 2 hr, adding the rest soda water, heating to 80 deg.C, and extracting for 30min to obtain water extractive solution and residue;

(2) soaking the residue in 60% ethanol solution 4 times the volume of the residue for 2 hr, heating under reflux at 90 deg.C for 3 hr, concentrating under reduced pressure at 75 deg.C to-0.08 Mpa, drying at 60 deg.C in vacuum drying oven to remove ethanol to obtain cortex Ilicis Rotundae ethanol extract;

(3) dissolving menthol in ethanol to obtain menthol solution;

Example 5

12 parts of ovateleaf holly bark, 1 part of aloe extract, 2 parts of chamomile extract, 0.2 part of citric acid, 0.3 part of edible spice, 1 part of xylitol, 1 part of menthol and 2 parts of ethanol; 80 parts of soda water.

(1) pulverizing cortex Ilicis Rotundae to 80 mesh, adding half of soda water, extracting at 50 deg.C for 2 hr, adding the rest soda water, heating to 80 deg.C, and extracting for 20min to obtain water extractive solution and residue;

(2) soaking the residue in 4 times volume of 50% ethanol solution for 1 hr, heating under reflux at 90 deg.C for 3 hr, concentrating under reduced pressure at 60 deg.C to-0.07 Mpa, vacuum drying at 60 deg.C to remove ethanol to obtain cortex Ilicis Rotundae ethanol extract;

(3) dissolving menthol in ethanol to obtain menthol solution;

Example 6

13 parts of ovateleaf holly bark, 2 parts of aloe extract, 1 part of chamomile extract, 0.3 part of citric acid, 0.1 part of edible spice, 1.5 parts of xylitol, 2 parts of menthol and 3 parts of ethanol; 85 parts of soda water.

(3) dissolving menthol in ethanol to obtain menthol solution;

Comparative example 1

Compared with the example 2, the composition total amount of the ovateleaf holly bark mouthwash is unchanged, and 1 part of aloe extract and 1 part of chamomile extract are replaced by 2 parts of chamomile extract;

11 parts of ovateleaf holly bark, 2 parts of chamomile extract, 0.2 part of citric acid, 0.3 part of edible spice, 1.5 parts of xylitol, 1 part of menthol and 2 parts of ethanol; 82 parts of soda water.

(3) dissolving menthol in ethanol to obtain menthol solution;

Comparative example 2

Compared with the example 2, the composition total amount of the rotunda officinalis mouthwash is unchanged, and 1 part of the aloe extract and 1 part of the chamomile extract are replaced by 2 parts of the aloe extract;

11 parts of ovateleaf holly bark, 2 parts of aloe extract, 0.2 part of citric acid, 0.3 part of edible spice, 1.5 parts of xylitol, 1 part of menthol and 2 parts of ethanol; 82 parts of soda water.

(3) dissolving menthol in ethanol to obtain menthol solution;

Comparative example 3

Compared with the embodiment 2, the difference is that: only one soda water extraction is carried out;

(1) pulverizing cortex Ilicis Rotundae to 70 mesh, adding soda water, extracting at 60 deg.C for 1.5 hr, heating to 75 deg.C, and extracting for 25min to obtain water extractive solution and residue;

(3) dissolving menthol in ethanol to obtain menthol solution;

Comparative example 4

Compared with the example 2, the difference is that the soda water is changed into distilled water;

11 parts of ovateleaf holly bark, 1 part of aloe extract, 1 part of chamomile extract, 0.2 part of citric acid, 0.3 part of edible spice, 1.5 parts of xylitol, 1 part of menthol and 2 parts of ethanol; and 82 parts of distilled water.

(1) pulverizing cortex Ilicis Rotundae to 70 mesh, adding half amount of distilled water, extracting at 60 deg.C for 1.5 hr, adding the rest distilled water, heating to 75 deg.C, and extracting for 25min to obtain water extractive solution and residue;

(3) dissolving menthol in ethanol to obtain menthol solution;

Comparative example 5

Compared with example 2, no citric acid is contained;

11 parts of ovateleaf holly bark, 1 part of aloe extract, 1 part of chamomile extract, 0.3 part of edible spice, 1.5 parts of xylitol, 1 part of menthol and 2 parts of ethanol; 82 parts of soda water.

(3) dissolving menthol in ethanol to obtain menthol solution;

Effect test

1. Verification of effects of cleaning oral cavity and refreshing breath

The subject was allowed to use a commercially available ordinary mouthwash and the rotunda rinse prepared in example 2, and the efficacy of the rotunda rinse was judged based on the sensory score. Randomly selecting 10 classmates with halitosis and 10 classmates which have just eaten garlic from college students, dividing the classmates into two groups, selecting 10 classmates with sensitive smell and no halitosis as assessors, and performing the following steps according to requirements:

(1) the testee directly converses with the assessor face-to-face at 0.5 m, and tests whether halitosis or garlic smell exists or not;

(2) after gargling with ordinary mouthwash for 2 minutes, the testers were in direct face-to-face conversation with the panelists at 0.5 m, and examined for the presence of halitosis or garlic odor;

(3) after 24h, the rotunda officinalis gargle is tested, so that the testers can directly talk with the assessors in a face-to-face manner at 0.5 m after gargling with the rotunda officinalis for 2 minutes, and the testers can check whether halitosis or garlic smell exists

The panelists scored the testers according to the fine scores (fresh breath, no peculiar smell 80-100 points in conversation, fresh breath, slight peculiar smell 79-60 points in conversation, slight peculiar smell in conversation, obvious improvement of 59-40 points in conversation, obvious peculiar smell in conversation, slightly improvement of 39-20 points in conversation, obvious peculiar smell in conversation, no improvement of 19-0 points in conversation). The scoring results are shown in table 1.

TABLE 1 mouthwash changes before and after rinsing mouth clean and fresh breath

The results in table 1 show that the invention adds the pure natural ovate leaf holly bark into the mouthwash, so that the mouthwash has the functions of cleaning the oral cavity and refreshing breath.

2. Verification of bacteriostatic effect

The sterilization effect test method comprises the following steps: the product is obtained by mixing (1-5). times.10⁴cfu/g of the bacterial solution was uniformly coated on the plate, and then the mouthwashes prepared in examples 2 to 6 and comparative examples 1 to 5 were uniformly coated on the surface of the plate; the incubation time was 5min, and the number of viable bacteria (in cfu/g) on the plate was measured and compared with the number of bacteria in the original bacterial solution to obtain the sterilization rate (%).

TABLE 2 Sterilization Rate (%)

The result shows that the mouthwash prepared by the invention has good sterilization effect.

3. Anti-inflammatory test

90 Kunming mice with the weight of 200 plus or minus 20 g; randomly divided into 9 groups, namely a model group, a blank control group (normal saline), examples 2-3 and comparative examples 1-5; spraying for administration, 1 time per day for 5 days, smearing 50 μ L of xylene on front and back surfaces of left ear of mouse 1h after last administration, taking right ear as control, removing neck of mouse after 2h, killing, cutting two ears along auricle base line, punching round ear piece at the same position with 9mm puncher, weighing, and taking difference between left and right ear pieces as swelling degree; the results of the experiment are shown in table 3 below:

TABLE 3 inhibition effect data sheet

Test group	Swelling degree (mg)
		Model set	18.2±2.3^c
Blank control group	16.9±4.7^a
		Example 2	10.6±3.1^b
Example 3	10.8±2.7^b
		Comparative example 1	13.6±3.8^a
Comparative example 2	15.4±4.9^a
		Comparative example 3	13.2±5.2^a
Comparative example 4	12.1±3.4^a
		Comparative example 5	14.5±6.6^a

Remarking: the different letters of a, b and c represent significant differences (p < 0.05);

the result shows that the mouthwash prepared by the invention has better anti-inflammatory effect.

The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.

Claims

1. The rotunda officinalis mouthwash is characterized by comprising the following raw materials: 8-13 parts of ovateleaf holly bark, 1-3 parts of aloe extract, 1-3 parts of chamomile extract, 0.1-0.5 part of citric acid, 0.1-0.5 part of edible spice, 1-2 parts of xylitol, 0.5-2 parts of menthol, 1-3 parts of ethanol and 75-90 parts of soda water;

the preparation method of the mouthwash is characterized by comprising the following steps:

(3) dissolving menthol in ethanol to obtain menthol solution;

2. The mouthwash according to claim 1, wherein the raw materials of the mouthwash consist of the following components in parts by weight: 12-13 parts of ovateleaf holly bark, 1-2 parts of aloe extract, 1-2 parts of chamomile extract, 0.2-0.3 part of citric acid, 0.1-0.3 part of edible spice, 1-1.5 parts of xylitol, 1-2 parts of menthol and 2-3 parts of ethanol; 80-85 parts of soda water.

3. A process for the preparation of a mouthwash according to any of claims 1 to 2, comprising the following steps:

(3) dissolving menthol in ethanol to obtain menthol solution;

4. The method for preparing mouthwash according to claim 3, wherein in step (1), the ovate leaf holly bark has a crushing mesh size of 60-80 meshes.

5. The process for preparing a mouthwash according to claim 3, wherein in step (1), the extraction is carried out at 50-70 ℃ for 1-2 h; the continuous extraction is carried out at 75-80 deg.C for 20-30 min.

6. The method for preparing mouthwash according to claim 3, wherein in the step (2), the volume of the ethanol is 3-4 times of the volume of the residue, and the concentration of the ethanol is 50-60%.

7. The process for preparing a mouthwash according to claim 3, wherein in step (2), the heating reflux is carried out at 85-90 ℃ for 2-3 h.

8. The process for preparing a mouthwash according to claim 3, wherein in step (2), the concentration under reduced pressure is carried out at 60-75 ℃, -0.06-0.08 MPa; the drying is carried out in a vacuum drying oven, and the temperature of the vacuum drying oven is set to be 40-60 ℃.