Mouthwash containing agilawood extract and preparation method thereof

Abstract

The invention discloses mouthwash containing agilawood extract and a preparation method of the mouthwash, and particularly belongs to the technical field of oral cleaning and nursing materials. The mouthwash is prepared from the following components: a composition containing an agilawood extract, a cosolvent, a flavoring agent and a solvent, the composition containing the agilawood extract comprises 5.3 to 7.6 parts of the agilawood extract, 1.1 to 2.5 parts of a cortex dictamni extract, 1.6 to 3.1 parts of a boxthorn root bark extract and 10.0 to 15.0 parts of oriental cherry water. The composition composed of the agilawood extract, the dictamnus dasycarpus root and bark extract, the boxthorn root and bark extract and the oriental cherry water provided by the invention has an excellent effect of inhibiting the growth of harmful bacteria in the oral cavity; the mouthwash provided by the invention can significantly reduce the production of methyl mercaptan after being co-cultured with saliva for 12 hours, which indicates that the mouthwash has the effects of freshening breath, reducing ozostomia and removing breath for 12 hours.

Description

Technical Field

[0001] The invention belongs to the technical field of oral cleaning and care products, and particularly relates to a mouthwash containing agarwood extract and a preparation method thereof. Background Art

[0002] Halitosis is a symptom of bad breath in the mouth, which is the odor emitted from the mouth or other gas-filled cavities such as the nose, sinuses, and pharynx. Halitosis is classified into true halitosis, false halitosis, and odontophobia according to international standards. The halitosis we refer to in our daily lives usually refers to true halitosis. The latter two categories (false halitosis and odontophobia) are generally believed to be non-existent and are mainly caused by psychological factors.

[0003] True halitosis can be divided into physiological halitosis and pathological halitosis. Pathological halitosis can be divided into oral halitosis and non-oral halitosis. The cause of oral halitosis is mainly the metabolites produced by the decomposition of sulfur-containing amino acids by microorganisms in the oral cavity (mainly Gram-negative anaerobic bacteria), and the products are mostly volatile sulfides. Current research shows that 85% to 90% of halitosis originates from the oral cavity. Using oral cleaning and care products to clean the oral cavity is the main method to remove common halitosis.

[0004] Chinese patent CN114288220A discloses an agarwood antibacterial gargle liquid, which includes agarwood extract, distilled water, seaweed extract, xylitol, vitamin B6 and edible essence. It has the characteristics of high antibacterial rate, no alcohol, pigment, fluoride, edible, etc., but the agarwood extract accounts for 15-90% of the overall formula, which is an ultra-high efficacy concentration mouthwash, which is extremely unfriendly to the oral cavity, has a strong agarwood flavor, is not suitable as a mouthwash for fresh breath, and has a high cost, which is not suitable for promotion and application.

[0005] Therefore, it is necessary to develop a mouthwash that can effectively freshen breath and remove bad breath, contains a lower concentration of agarwood extract and a compound of antibacterial agents from multiple natural plant extracts. The mouthwash can effectively reduce the number of periodontal pathogens that cause oral halitosis in the mouth, reduce the production of volatile sulfides such as methyl mercaptan, and achieve the effect of reducing bad breath and having a long-lasting fresh breath. Summary of the invention

[0006] In view of the deficiencies in the prior art, the object of the present invention is to provide a mouthwash that can effectively freshen breath, remove bad breath, contains a low concentration of agarwood extract, and is compounded with multiple natural plant extracts. The mouthwash can effectively reduce the number of periodontal pathogens that cause oral halitosis in the oral cavity according to the cause of oral halitosis, reduce the production of volatile sulfides such as methyl mercaptan, thereby reducing bad breath and having a long-lasting effect of freshening breath.

[0007] To achieve the above object, the present invention discloses the following technical solutions:

[0008] In a first aspect, the present invention provides a composition comprising an agarwood extract, wherein the composition comprises the following components in parts by mass:

[0009] Agarwood extract 5.3-7.6 parts;

[0010] 1.1-2.5 parts of Dictamni root bark extract;

[0011] 1.6-3.1 parts of wolfberry root bark extract;

[0012] 10.0-15.0 parts of Guanshan cherry blossom water.

[0013] Preferably, the composition comprises the following components in parts by mass:

[0014] 6.0-7.0 parts of agarwood extract;

[0015] 1.6-2.1 parts of Dictamni root bark extract;

[0016] 2.1-2.6 parts of wolfberry root bark extract;

[0017] 12.0-14.0 parts of Guanshan cherry blossom water.

[0018] Further preferably, the method for preparing the Guanshan cherry blossom water comprises the following steps:

[0019] S1-1. Take the dried cherry blossoms and crush them through a 60-mesh sieve to obtain cherry blossom powder;

[0020] S1-2. Take the cherry blossom powder obtained in step S1-1 and mix it with deionized water, the solid-liquid ratio is 1:10g / mL, and ultrasonic stirring is performed at a speed of 50r / min and an ultrasonic frequency of 28kHz for 20min to obtain a solid-liquid mixture;

[0021] S1-3. Heat the solid-liquid mixture obtained in step S1-2 to 60°C, keep warm for 10 hours, filter and remove the residue to obtain Guanshan cherry blossom water.

[0022] In a second aspect, the present invention provides the use of the above-mentioned composition containing agarwood extract in the preparation of oral cleaning and care products with antibacterial and antibacterial effects.

[0023] In a third aspect, the present invention provides a mouthwash comprising an agarwood extract, wherein the mouthwash comprises the composition described in the first aspect.

[0024] Preferably, the composition is added in an amount of 4-6 wt % in mouthwash.

[0025] Preferably, the mouthwash further comprises a solubilizing agent, a flavoring agent and a solvent.

[0026] Further preferably, the cosolvent is glycerol;

[0027] The flavoring agent is at least one of acesulfame potassium and menthol;

[0028] The solvent is deionized water.

[0029] In a fourth aspect, the present invention provides a method for preparing a mouthwash comprising an agarwood extract according to the third aspect, comprising the following steps:

[0030] S2-1. First, take glycerol, menthol and 1 / 5 of the total amount of deionized water, mix and stir at 100r / min to dissolve evenly to obtain a mixed solution A;

[0031] S2-2. Take acesulfame potassium and 1 / 10 of the total amount of deionized water and mix and dissolve evenly to obtain a mixed solution B;

[0032] S2-3. The composition containing the agarwood extract, the mixed solution A, the mixed solution B and the remaining deionized water are mixed and stirred at 200 r / min to obtain the mouthwash containing the agarwood extract.

[0033] In the present invention:

[0034] Agarwood extract contains a variety of chemical components, including monoterpenes, sesquiterpenes, diterpenes, triterpenes, sterols, flavonoids, benzylacetone, chromones, phenolic acids and aliphatic compounds, which can effectively improve the balance of oral flora, reduce the growth of harmful bacteria, promote oral health, and prevent oral diseases such as gingivitis and periodontal disease. Agarwood extract also has a certain analgesic effect and can relieve pain caused by oral problems.

[0035] Lycium barbarum root bark extract is rich in a variety of chemical components, including alkaloid compounds, organic acids, ester compounds, phenylpropanoid compounds, anthraquinone compounds and other chemical components, which endow Lycium barbarum root bark extract with a variety of potential pharmacological activities. In mouthwash, Lycium barbarum root bark extract has antibacterial, anti-inflammatory, antipyretic and analgesic effects, which helps to reduce oral bacteria, reduce oral inflammation and relieve oral pain. In addition, Lycium barbarum root bark extract may also play an indirect benefit by improving the oral environment and promoting oral health.

[0036] The root bark extract of Dictamni contains rich chemical components, such as alkaloids, lactone compounds, sitosterol, quercetin, berberine, berberine acid, fatty acids and crude saponins, which can effectively reduce oral bacteria, reduce dental plaque adhesion, and prevent gingivitis and caries; at the same time, the root bark extract of Dictamni can reduce oral inflammation and gingival swelling and pain through anti-inflammatory effects, thereby reducing the sensitive response of gums.

[0037] Guanshan cherry blossom water is rich in total flavonoids, polyphenol compounds, vitamin C, amino acids, polysaccharides, organic acids, natural vitamin A, vitamin B, vitamin E and other active ingredients. These ingredients have good antioxidant effects, help to remove free radicals in the mouth, reduce cell damage, and also have antibacterial and anti-inflammatory activity, which helps to reduce harmful bacteria in the mouth, prevent periodontal disease and oral ulcers, while freshening breath and improving bad breath.

[0038] The present invention has found that the combination of agarwood extract, Dictamni root bark extract, wolfberry root bark extract and Prunus guanshanensis water can effectively reduce the number of periodontal pathogens in the oral cavity that cause oral halitosis, thereby reducing the production of volatile sulfides such as methyl mercaptan, thereby achieving the effect of reducing halitosis and having a long-lasting fresh breath.

[0039] Beneficial effects of the present invention:

[0040] 1. The composition composed of agarwood extract, Dictamni root bark extract, Lycium bark root bark extract and Prunus guanshanensis water provided by the present invention has excellent effect of inhibiting the growth of harmful bacteria in the oral cavity.

[0041] 2. The mouthwash provided by the present invention can significantly reduce the production of methyl mercaptan after being co-incubated with saliva for 12 hours, indicating that it has the effects of refreshing breath, reducing bad breath and removing bad breath for 12 hours. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 The fresh breath test data and statistical analysis chart; among them, * indicates significant difference, P < 0.05, ** indicates extremely significant difference, P < 0.01. DETAILED DESCRIPTION

[0043] The present invention will be further described below in conjunction with specific examples. These examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. The following examples are implementation methods with specific conditions noted, usually according to conventional conditions or according to the conditions recommended by the manufacturer.

[0044] Unless otherwise defined, all professional and scientific terms used herein have the same meanings as those known to those skilled in the art. In addition, any methods and materials similar or equivalent to those described herein can be applied to the methods of the present invention. The preferred implementation methods and materials described herein are for demonstration purposes only.

[0045] In the present invention:

[0046] Agarwood extract: purchased from Fufeng Snot Biotechnology Co., Ltd., specification 20:1, water-soluble powder;

[0047] Lycium barbarum root bark extract: also known as Lycium bark bark extract, purchased from Xi'an An'ao Biotechnology Co., Ltd., specification 10:1, water-soluble powder;

[0048] Dictamni root bark extract: purchased from Xi'an Changyue Biotechnology Co., Ltd., specification 10:1, water-soluble powder;

[0049] Guanshan cherry: a plant belonging to the genus Prunus of the Rosaceae family, with the Latin name Prunus serrulata'Sekiyama', purchased from Yangzhou Huaersi Food Co., Ltd.

[0050] Other raw materials involved in the present invention can be purchased through commercial channels.

[0051] Preparation of Guanshan cherry blossom water:

[0052] Step S1-1, taking dried cherry blossoms from Guanshan Mountain and crushing them in a universal high-speed grinder, and passing them through a 60-mesh sieve to obtain cherry blossom powder;

[0053] Step S1-2, mixing the cherry blossom powder and deionized water in step S1-1 at a solid-liquid ratio of 1:10 g / mL, and performing ultrasonic stirring treatment at a speed of 50 r / min and an ultrasonic frequency of 28 kHz for 20 min to obtain a solid-liquid mixture;

[0054] Step S1-3, then heat the solid-liquid mixture to 60°C, keep it warm for 10 hours, and finally filter out the residue to obtain Guanshan cherry blossom water.

[0055] Preparation of a composition comprising agarwood extract:

[0056] The raw materials in Table 1 are accurately weighed according to their mass fractions, placed in a high-speed homogenizer and mixed and dispersed evenly to obtain a composition containing agarwood extract.

[0057] Table 1 Composition raw materials weight parts

[0058]

[0059] Note: “-” in the table means no addition.

[0060] The above compositions 1-13 were mixed with deionized water respectively and stirred evenly, wherein the mass ratio of the composition to the deionized water was 1:19, to obtain a solution with a concentration of 5 wt %, which was used as a test sample for the antibacterial test.

[0061] Antibacterial test

[0062] Bacterial strains: Staphylococcus aureus GDMCC NO.: 1.1220, Porphyromonas gingivalis GDMCC NO.: 1.851, Candida albicans GDMCC NO.: 2.178, all purchased from Guangdong Microbiological Culture Collection Center.

[0063] For Staphylococcus aureus, nutrient agar slants and nutrient agar medium were used;

[0064] Porphyromonas gingivalis was cultured on TSA slants and TSA medium;

[0065] Candida albicans was cultured on Sabouraud agar slant and Sabouraud agar medium.

[0066] Preparation of bacterial suspension: Take fresh slant bacteria cultured on agar slant for 18-24 hours, wash the slant bacteria with PBS and dilute to 1×10 4 ~9×10 4 CFU / mL bacterial suspension. The bacterial suspension should be used within 2 hours if placed at room temperature. If stored at 2-8°C, it can be used within 24 hours.

[0067] Sample preparation: The test sample was prepared by making the above-prepared compositions 1-13 into solutions with a concentration of 5 wt %, and the control sample was a PBS solution.

[0068] Test method: Take 0.1mL of bacterial suspension and add it to a test tube containing 5mL of sample solution, quickly mix it into a mixed solution, and start timing immediately. The action time is 5 minutes. After the predetermined time, take 0.5mL of the mixed solution and add it to 4.5mL of PBS solution, and mix it thoroughly to form a sample solution; take 1mL of the sample solution (or dilute it appropriately, such as taking 2 to 3 dilutions) and place it in a sterile plate. Inoculate two plates with each sample solution, pour 20mL of agar culture medium cooled to 40 to 45℃, rotate the plate to make it fully uniform, turn the plate over after the agar solidifies, and culture it at (35±2)℃ for 48h. C. albicans culture it for 72h, and count the live bacteria.

[0069] The antibacterial rate calculation formula is:

[0070]

[0071] Where:

[0072] X——inhibition rate (%);

[0073] A0——average colony count of control samples;

[0074] A1——The average colony count of the test sample, the antibacterial rate result is rounded to one decimal place.

[0075] The specific antibacterial rate results are shown in Table 2.

[0076] Table 2 Antibacterial rate results

[0077]

[0078] Result analysis:

[0079] According to WS / T 650-2019 "Antibacterial and Antibacterial Effect Evaluation Method", when the antibacterial rate is ≥50% to 90%, it has an antibacterial effect, and when the antibacterial rate is ≥90%, it has a strong antibacterial effect; the composition composed of agarwood extract, Dictamni root bark extract, Lycium bark root bark extract and Prunus kansana water provided by the present invention has excellent effect of inhibiting the growth of harmful bacteria in the oral cavity.

[0080] Preparation of mouthwash:

[0081] Weigh the raw materials according to Table 3;

[0082] Step S2-1, firstly mix glycerol, menthol and 1 / 5 deionized water, and mix and stir at 100 r / min to uniformly dissolve to obtain a mixed solution A;

[0083] Step S2-2, mixing acesulfame potassium with 1 / 10 deionized water and dissolving them uniformly to obtain a mixed solution B;

[0084] Step S2-3, mixing and stirring the composition, mixed solution B, mixed solution A and the remaining deionized water at 200 r / min to obtain mouthwash examples 1-3 and comparative examples 1-2.

[0085] Table 3 Mouthwash raw material mass percentage

[0086]

[0087] Note: “-” in the table means no addition.

[0088] Fresh breath test

[0089] 1 Experimental Grouping

[0090] Sample group: mouthwashes of Examples 1-3 and Comparative Example 1;

[0091] Blank control group: mouthwash of comparative example 2 (without effective ingredients);

[0092] Positive control group: the mouthwash of Comparative Example 3.

[0093] 2 Experimental methods

[0094] 2.1 Preparation of saliva: A total of 50 g of saliva was collected from 8 volunteers and placed in a 120 mL centrifuge tube. The tube was then centrifuged at 8000 r / min for 15 min and the supernatant was collected.

[0095] 2.2 Overnight culture (film formation): Take 30 10mL centrifuge tubes, put a hydroxyapatite (HAP) sheet in each centrifuge tube and add 1mL of saliva supernatant, then place the centrifuge tube in a constant temperature water bath at 37℃ for overnight culture to form an acquired biofilm on the surface of the HAP sheet. The next day, take the centrifuge tube out of the water bath and aspirate the saliva in the tube.

[0096] 2.3 Sample preparation: directly take the above-prepared Examples 1-3 and Comparative Examples 1-2 and commercially available Listerine mouthwash (Ice Blue Zero Mouthwash) for use.

[0097] 2.4 Treatment of test samples: 30 cultured HAP sheets were randomly divided into a sample group and a control group, with 5 sheets in each group. The HAP sheets in the sample group were soaked in the mouthwashes of Examples 1-3 and Comparative Example 1 for 30 seconds, taken out and placed in headspace bottles, with 1 sheet in each bottle; the blank control group and the positive control group were treated in the same manner with the mouthwash of Comparative Example 2 and the commercially available Listerine mouthwash (Ice Blue Zero Mouthwash), respectively.

[0098] 2.5 Preparation of saliva culture medium solution: Weigh 0.75g of thioglycollate culture medium, add 25g of deionized water, heat and stir to dissolve as culture medium stock solution. Collect 100g of saliva from 8 volunteers and store it in a centrifuge tube. Weigh a certain weight of culture medium stock solution, deionized water and saliva according to the mass ratio of 1.6:13.4:85 (culture medium stock solution: deionized water: saliva), mix well and obtain saliva culture medium solution for use.

[0099] 2.6 Overnight culture (volatile sulfide): Add 3 mL of saliva culture medium solution to each headspace bottle, and then place it in a constant temperature water bath at 37°C for overnight culture (12 hours) to produce volatile sulfide. Take the cultured headspace bottle out of the water bath the next day.

[0100] 2.7 Detection of the amount of methyl mercaptan produced: methyl mercaptan is one of the characteristic substances of breath. The smaller the detection value, the less methyl mercaptan is, indicating that the breath is fresher. Place the headspace bottle in the headspace sampler and obtain the peak area of ​​methyl mercaptan by gas chromatography-flame photometric detector GC-FPD.

[0101] 2.8 Evaluation method: After taking the logarithm of the peak area of ​​the sample group and the control group, the t-test was performed using SPSS27.0 statistical software, with a significant difference level of α = 0.05. If the sample group value is less than the blank control group value and there is a statistical difference (P < 0.05), it means that the sample group can significantly reduce the production of methyl mercaptan after 12 hours of co-culture with saliva, and has the effect of refreshing breath.

[0102] 3. Test data and statistical results

[0103] 3.1 Test data and statistical results are shown in Table 4 and Figure 1 .

[0104] Table 4 Fresh breath test data

[0105]

[0106]

[0107] 4 Conclusion Analysis

[0108] Compared with the blank control group, Examples 1-3 in the sample group can significantly reduce the production of methyl mercaptan after being co-cultured with saliva for 12 hours, indicating that the mouthwashes of Examples 1-3 have the effects of freshening breath, reducing bad breath, and reducing bad breath.

[0109] Compared with the positive control group, Examples 1-3 in the sample group have similar performances as the commercially available breath freshening mouthwash in freshening breath and reducing bad breath, and can significantly reduce the production of methyl mercaptan.

[0110] Compared with Comparative Example 1, Example 2 has significantly better performance in reducing bad breath and refreshing breath than Comparative Example 1, indicating that the effective ingredients composed of agarwood extract, Dictamni root bark extract, Lycium bark root bark extract and Prunus kansana water are the key effective components for reducing bad breath and refreshing breath.

[0111] Although there is no significant difference between Examples 1-3, it can be seen from the logarithmic mean that as the concentration of the composition increases, the production of methyl mercaptan gradually decreases, indicating a certain concentration dependence. As the concentration of the composition increases, the performance of the mouthwash in freshening breath and reducing bad breath gradually increases, which also shows that the effective ingredients composed of agarwood extract, Dictamni root bark extract, Lycium bark root bark extract and Prunus guanshanensis water are the key effective components for reducing bad breath and freshening breath in the mouthwash provided by the present invention.

[0112] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A composition comprising an agarwood extract, characterized in that: The composition comprises the following components in parts by mass: Agarwood extract 5.3-7.6 parts; 1.1-2.5 parts of Dictamni root bark extract; 1.6-3.1 parts of wolfberry root bark extract; 10.0-15.0 parts of Guanshan cherry blossom water.

2. The composition comprising agarwood extract according to claim 1, characterized in that The composition comprises the following components in parts by mass: 6.0-7.0 parts of agarwood extract; 1.6-2.1 parts of Dictamni root bark extract; 2.1-2.6 parts of wolfberry root bark extract; 12.0-14.0 parts of Guanshan cherry blossom water.

3. The composition comprising agarwood extract according to claim 2, characterized in that The preparation method of the Guanshan cherry blossom water comprises the following steps: S1-1. Take the dried cherry blossoms and crush them through a 60-mesh sieve to obtain cherry blossom powder; S1-2. Take the cherry blossom powder obtained in step S1-1 and mix it with deionized water, the solid-liquid ratio is 1:10g / mL, and ultrasonic stirring is performed at a speed of 50r / min and an ultrasonic frequency of 28kHz for 20min to obtain a solid-liquid mixture; S1-3. Heat the solid-liquid mixture obtained in step S1-2 to 60°C, keep warm for 10 hours, filter and remove the residue to obtain Guanshan cherry blossom water.

4. Use of the composition containing agarwood extract according to any one of claims 1 to 3 in the preparation of oral cleaning and care products with antibacterial and antibacterial effects.

5. A mouthwash containing agarwood extract, characterized in that: The mouthwash comprises the composition comprising the agarwood extract according to any one of claims 1 to 3.

6. The mouthwash containing agarwood extract according to claim 5, characterized in that The composition containing the agarwood extract is added in an amount of 4-6 wt % in the mouthwash.

7. The mouthwash containing agarwood extract according to claim 5, characterized in that The mouthwash also comprises a solubilizing agent, a flavoring agent and a solvent.

8. The mouthwash containing agarwood extract according to claim 7, characterized in that The cosolvent is glycerol; The flavoring agent is at least one of acesulfame potassium and menthol; The solvent is deionized water.

9. A method for preparing a mouthwash containing agarwood extract according to claim 7, characterized in that: The following steps are involved: S2-1. First, take glycerol, menthol and 1 / 5 of the total amount of deionized water, mix and stir at 100r / min to dissolve evenly to obtain a mixed solution A; S2-2. Take acesulfame potassium and 1 / 10 of the total amount of deionized water and mix and dissolve evenly to obtain a mixed solution B; S2-3. The composition containing the agarwood extract, the mixed solution A, the mixed solution B and the remaining deionized water are mixed and stirred at 200 r / min to obtain the mouthwash containing the agarwood extract.

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