A mouthwash comprising an extract of agarwood and a method of preparing the same

Abstract

This invention discloses a mouthwash containing agarwood extract and its preparation method, specifically belonging to the technical field of oral hygiene products. The mouthwash comprises the following components: a composition containing agarwood extract, a solubilizer, a flavoring agent, and a solvent. The composition containing agarwood extract includes 5.3-7.6 parts agarwood extract, 1.1-2.5 parts Dictamnus dasycarpus root bark extract, 1.6-3.1 parts Lycium barbarum root bark extract, and 10.0-15.0 parts Kanzan cherry blossom water. The composition of agarwood extract, Dictamnus dasycarpus root bark extract, Lycium barbarum root bark extract, and Kanzan cherry blossom water provided by this invention has excellent inhibitory effects on the growth of harmful bacteria in the oral cavity. After 12 hours of co-culturing with saliva, the mouthwash provided by this invention significantly reduces the production of methanethiol, indicating that it has the effects of freshening breath, reducing halitosis, and eliminating bad breath for 12 hours.

Description

Technical Field

[0001] This invention belongs to the technical field of oral hygiene products, specifically relating to a mouthwash containing agarwood extract and its preparation method. Background Technology

[0002] Halitosis, or bad breath, is a symptom of unpleasant odor emanating from the mouth or other air-filled cavities such as the nose, sinuses, and pharynx. According to international standards, halitosis is classified into true halitosis, pseudo-halitosis, and malodoremia. In everyday life, the halitosis we usually refer to is true halitosis. The latter two types (pseudo-halitosis and malodoremia) are generally considered to be non-existent and primarily caused by psychological factors.

[0003] True halitosis can be divided into physiological halitosis and pathological halitosis. Pathological halitosis can be further divided into oral halitosis and non-oral halitosis. The cause of oral halitosis is mainly the metabolic products produced by the decomposition of sulfur-containing amino acids by oral microorganisms (mainly Gram-negative anaerobic bacteria), and these products are mostly volatile sulfur compounds. Current research shows that 85% to 90% of halitosis originates from the oral cavity, and using oral hygiene products to clean the mouth is the main method for eliminating common halitosis.

[0004] Chinese patent CN114288220A discloses an agarwood mouthwash with antibacterial properties, comprising agarwood extract, distilled water, seaweed extract, xylitol, vitamin B6, and edible flavoring. It boasts a high antibacterial rate, is free of alcohol, pigments, and fluoride, and is edible. However, the agarwood extract constitutes 15-90% of the overall formula, making it an extremely high-concentration mouthwash that is very unfriendly to the oral cavity. Its strong agarwood aroma makes it unsuitable as a breath freshener, and its high cost limits its widespread application.

[0005] Therefore, it is necessary to develop a mouthwash that can effectively freshen breath and eliminate bad breath, containing a low concentration of agarwood extract and a variety of natural plant extracts as antibacterial agents. This mouthwash can effectively reduce the number of periodontal pathogens that cause oral halitosis in the mouth, reduce the production of volatile sulfur compounds such as methanethiol, and achieve the effect of reducing bad breath and providing long-lasting fresh breath. Summary of the Invention

[0006] In view of the shortcomings of the prior art, the purpose of this invention is to provide a mouthwash that can effectively freshen breath, eliminate halitosis, contains a low concentration of agarwood extract, and is compounded with a variety of natural plant extracts. Based on the etiology of oral halitosis, this mouthwash can effectively reduce the number of periodontal pathogens that cause oral halitosis in the oral cavity, reduce the production of volatile sulfur compounds such as methanethiol, and achieve the effect of reducing halitosis and providing long-lasting fresh breath.

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

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

[0009] Agarwood extract 5.3-7.6 parts;

[0010] Dictamnus dasycarpus root bark extract 1.1-2.5 parts;

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

[0012] Kanzan cherry blossom water, 10.0-15.0 servings.

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

[0014] Agarwood extract 6.0-7.0 parts;

[0015] Dictamnus dasycarpus root bark extract 1.6-2.1 parts;

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

[0017] Kanzan Cherry Blossom Water, 12.0-14.0 servings.

[0018] More preferably, the preparation method of the Guanshan cherry blossom water includes the following steps:

[0019] S1-1. Take dried cherry blossoms from Kanzan, grind them into powder, and pass 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 deionized water, with a material-to-liquid ratio of 1:10 g / mL, and perform ultrasonic stirring at a speed of 50 r / min and an ultrasonic frequency of 28 kHz for 20 min to obtain a solid-liquid mixture.

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

[0022] Secondly, the present invention provides the application of the above-mentioned composition containing agarwood extract in the preparation of oral hygiene products with antibacterial and bacteriostatic effects.

[0023] Thirdly, the present invention provides a mouthwash containing agarwood extract, wherein the mouthwash contains the composition described in the first aspect.

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

[0025] Preferably, the mouthwash further includes a solubilizer, a flavoring agent, and a solvent.

[0026] More 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] Fourthly, the present invention provides a method for preparing the mouthwash containing agarwood extract as described in the third aspect, comprising the following steps:

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

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

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

[0033] In this invention:

[0034] Agarwood extract contains a variety of chemical components, including monoterpenes, sesquiterpenes, diterpenes, triterpenes, sterols, flavonoids, benzylacetone, crromones, phenolic acids, and aliphatic compounds. It 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 periodontitis. Agarwood extract also has a certain analgesic effect and can relieve pain caused by oral problems.

[0035] Lycium bark extract is rich in various chemical components, including alkaloids, organic acids, esters, phenylpropanoids, anthraquinones, and other chemical compounds. These components endow Lycium bark extract with a variety of potential pharmacological activities. In mouthwash, Lycium bark extract has antibacterial, anti-inflammatory, antipyretic, and analgesic effects, helping to reduce oral bacteria, alleviate oral inflammation, and relieve oral pain. Furthermore, Lycium bark extract may also exert indirect benefits by improving the oral environment and promoting oral health.

[0036] Dictamnus dasycarpus root bark extract contains abundant chemical components, such as alkaloids, lactones, sitosterol, quercetin, berberine, berberine acid, fatty acids, and crude saponins. These components can effectively reduce oral bacteria, reduce plaque buildup, and prevent gingivitis and tooth decay. At the same time, Dictamnus dasycarpus root bark extract can alleviate oral inflammation and gingival swelling and pain through its anti-inflammatory effects, thereby reducing gingival sensitivity.

[0037] Kanzan cherry blossom water contains abundant total flavonoids, polyphenols, vitamin C, amino acids, polysaccharides, organic acids, natural vitamin A, vitamin B, vitamin E and other active ingredients. These ingredients have good antioxidant effects, which help to remove free radicals in the mouth and reduce cell damage. They also have antibacterial and anti-inflammatory activities, which help to reduce harmful bacteria in the mouth, prevent periodontal disease and oral ulcers, and freshen breath and improve bad breath.

[0038] This invention has found that when agarwood extract, Dictamnus dasycarpus root bark extract, Lycium barbarum root bark extract, and Cherry blossom water are used in combination, they can effectively reduce the number of periodontal pathogens that cause oral halitosis in the mouth, thereby reducing the production of volatile sulfur compounds such as methanethiol, thus achieving the effect of reducing halitosis and providing long-lasting fresh breath.

[0039] The beneficial effects of this invention are:

[0040] 1. The composition of agarwood extract, dictamnus root bark extract, wolfberry root bark extract and sakura water provided by the present invention has excellent effect in inhibiting the growth of harmful bacteria in the oral cavity.

[0041] 2. The mouthwash provided by this invention can significantly reduce the production of methanethiol after being co-cultured with saliva for 12 hours, indicating that it has the effects of freshening breath, reducing bad breath, and eliminating bad breath for 12 hours. Attached Figure Description

[0042] Figure 1 The data and statistical analysis charts for the breath freshening test are shown; where * indicates a significant difference (P < 0.05), and ** indicates an extremely significant difference (P < 0.01). Detailed Implementation

[0043] The present invention will be further illustrated below with reference to specific embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. The following embodiments are implementation methods to indicate specific conditions, generally performed under conventional conditions or as recommended by the manufacturer.

[0044] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those well known to those skilled in the art. Furthermore, any methods and materials similar to or equivalent to those described herein may be applied to the methods of this invention. The preferred embodiments and materials described herein are for illustrative purposes only.

[0045] In this invention:

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

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

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

[0049] Guanshan Cherry Blossom: A plant belonging to the genus Prunus of the family Rosaceae, with the Latin name Prunus serrulata 'Sekiyama', purchased from Yangzhou Huaershi Food Co., Ltd.;

[0050] All other raw materials involved in this invention are commercially available.

[0051] Preparation of Kanzan cherry blossom water:

[0052] Step S1-1: Take dried cherry blossoms from Kanzan, place them in a universal high-speed grinder and grind them, then pass them through a 60-mesh sieve to obtain cherry blossom powder;

[0053] Step S1-2: Take the cherry blossom powder and deionized water from step S1-1 and mix them at a ratio of 1:10 g / mL. Then, perform ultrasonic stirring at a speed of 50 r / min and an ultrasonic frequency of 28 kHz for 20 min to obtain a solid-liquid mixture.

[0054] Steps S1-3: Then heat the solid-liquid mixture to 60°C, keep it warm for 10 hours, and finally filter to remove the residue to obtain Kanzan cherry blossom water.

[0055] Preparation of compositions containing agarwood extract:

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

[0057] Table 1. Mass parts of raw materials for the composition

[0058]

[0059] Note: "-" in the table indicates no additions.

[0060] Take the above compositions 1-13 and mix them with deionized water until homogeneous. The mass ratio of the composition to the deionized water is 1:19. The resulting solution has a concentration of 5 wt% and is used as the test sample for the antibacterial test.

[0061] Antibacterial test

[0062] The bacterial strains were Staphylococcus aureus GDMCC NO. 1.1220, Porphyromonas gingivalis GDMCC NO. 1.851, and Candida albicans GDMCC NO. 2.178, all of which were purchased from the Guangdong Provincial Center for Microbial Culture Collection.

[0063] Staphylococcus aureus was cultured using nutrient agar slants and nutrient agar medium.

[0064] Porphyromonas gingivalis was cultured using TSA slant and TSA medium.

[0065] Candida albicans was prepared using Sabouraud agar slants and Sabouraud agar medium.

[0066] Preparation of bacterial suspension: Take fresh bacterial strains from agar slant cultured for 18–24 h, wash the slant strains with PBS and dilute to 1×10⁻⁶. 4 ~9×10 4 CFU / mL bacterial suspension. The bacterial suspension should be used within 2 hours when left at room temperature, or within 24 hours if stored at 2-8℃.

[0067] Sample preparation: The test sample was a 5 wt% solution of the above-prepared composition 1-13, and the control sample was a PBS solution.

[0068] Experimental method: Add 0.1 mL of bacterial suspension to a test tube containing 5 mL of sample solution, mix quickly to form a mixed solution, and start timing immediately. The reaction time is 5 min. After the predetermined time, add 0.5 mL of the mixed solution to 4.5 mL of PBS solution and mix thoroughly to form a sample solution. Take 1 mL of sample solution (or dilute appropriately, such as taking 2-3 dilutions) and place it in a sterile Petri dish. Inoculate two Petri dishes with each sample solution. Pour in 20 mL of agar medium cooled to 40-45℃, rotate the Petri dish to make it fully uniform, and after the agar solidifies, invert the Petri dish. Incubate at (35±2)℃ for 48 h. Incubate Candida albicans for 72 h and count the viable bacteria.

[0069] The formula for calculating the antibacterial rate is:

[0070]

[0071] In the formula:

[0072] X – Antibacterial rate (%);

[0073] A0—The average colony count of the control sample;

[0074] A1 represents the average number of colonies in the test sample, and the inhibition rate result is rounded to one decimal place.

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

[0076] Table 2. Results of antibacterial rate

[0077]

[0078] Results analysis:

[0079] According to WS / T 650-2019 "Evaluation Method for Antibacterial and Bacteriostatic Effects", 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 of agarwood extract, Dictamnus dasycarpus root bark extract, Lycium barbarum root bark extract and Cherry Blossom Water provided by this invention has excellent efficacy in 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: First, take glycerol, menthol and 1 / 5 deionized water and mix them at 100 r / min to dissolve them evenly to obtain mixed solution A;

[0083] Step S2-2: Mix acesulfame potassium with 1 / 10 deionized water and dissolve thoroughly to obtain mixed solution B;

[0084] Steps S2-3: Mix the composition, mixed solution B, mixed solution A and the remaining deionized water at 200 r / min until homogeneous to obtain mouthwash Examples 1-3 and Comparative Examples 1-2.

[0085] Table 3. Percentage of raw materials in mouthwash by weight

[0086]

[0087] Note: "-" in the table indicates no additions.

[0088] Fresh breath test

[0089] 1. Experimental Groups

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

[0091] Blank control group: mouthwash from Comparative Example 2 (without active ingredients);

[0092] Positive control group: mouthwash from control group 3.

[0093] 2 Experimental Methods

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

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

[0096] 2.3 Sample preparation: Take the samples prepared above, including Examples 1-3 and Comparative Examples 1-2, as well as commercially available Listerine mouthwash (Ice Blue Zero Mouthwash), for later use.

[0097] 2.4 Sample preparation: Thirty cultured HAP tablets were randomly divided into a sample group and a control group, with five tablets in each group. The HAP tablets in the sample group were immersed in the mouthwash of Examples 1-3 and Comparative Example 1 for 30 seconds, and then placed in headspace vials, one tablet per vial. The blank control group and the positive control group were treated in the same way 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 thioglycolate medium, add 25g of deionized water, heat and stir appropriately to dissolve, and use as the culture medium stock solution. Collect 100g of saliva from 8 volunteers and store it in centrifuge tubes. 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 to obtain the saliva culture medium solution for later use.

[0099] 2.6 Overnight culture (volatile sulfides): Add 3 mL of saliva culture medium solution to each headspace vial, and then incubate overnight (12 h) in a 37°C water bath to produce volatile sulfides. Remove the cultured headspace vials from the water bath the next day.

[0100] 2.7 Detection of Methanethiol Production: Methanethiol is one of the characteristic substances of bad breath. The lower the detection value, the less methanethiol is present, indicating fresher breath. The headspace vial is placed in a headspace sampler, and the peak area of ​​methanethiol is obtained by gas chromatography-flame photometry (GC-FPD).

[0101] 2.8 Evaluation Method: After taking the logarithm of the peak areas of the sample group and the control group, a t-test was performed using SPSS 27.0 statistical software, with a significance level of α = 0.05. If the value of the sample group was less than that of the blank control group and there was a statistically significant difference (P < 0.05), it indicated that the sample group, after 12 hours of co-culture with saliva, could significantly reduce the production of methanethiol and had a breath-freshening effect.

[0102] 3. Test data and statistical results

[0103] 3.1 The 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 and Analysis

[0108] Compared with the blank control group, the samples from Examples 1-3 showed a significant reduction in the production of methanethiol after 12 hours of co-culturing with saliva, indicating that the mouthwashes from Examples 1-3 have the effect of freshening breath, reducing halitosis, and eliminating bad breath for 12 hours.

[0109] Compared with the positive control group, Examples 1-3 in the sample group had similar breath freshening and halitosis-reducing performance to commercially available breath freshening mouthwashes, and all of them could significantly reduce the production of methanethiol.

[0110] Compared with Comparative Example 1, Example 2 showed significantly better performance in reducing and freshening breath than Comparative Example 1, indicating that the active ingredients composed of agarwood extract, Dictamnus dasycarpus root bark extract, Lycium barbarum root bark extract and Kanzan cherry blossom water are the key active ingredients for reducing and freshening breath.

[0111] Although there were no significant differences between Examples 1-3, the logarithmic mean showed that the production of methanethiol gradually decreased with increasing composition concentration, indicating a certain concentration dependence. As the composition concentration increased, the mouthwash's ability to freshen breath and reduce halitosis gradually improved. This also demonstrates that the active ingredients composed of agarwood extract, dictamnus root bark extract, wolfberry root bark extract, and cherry blossom water are key active ingredients for reducing and freshening breath in the mouthwash provided by this invention.

[0112] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A composition comprising an extract of Aquilaria agallocha, characterized in that, The composition comprises the following components in parts by weight: Agarwood extract 6.0-7.0 parts; Dictamnus dasycarpus root bark extract 1.6-2.1 parts; 2.1-2.6 parts of wolfberry root bark extract; Kanzan cherry blossom water, 12.0-14.0 servings; The preparation method of the Guanshan cherry blossom water includes the following steps: S1-1. Take dried cherry blossoms from Kanzan, grind them into powder, and pass them through a 60-mesh sieve to obtain cherry blossom powder; S1-2. Take the cherry blossom powder obtained in step S1-1 and deionized water, with a material-to-liquid ratio of 1:10 g / mL, and perform ultrasonic stirring at a speed of 50 r / min and an ultrasonic frequency of 28 kHz for 20 min to obtain a solid-liquid mixture. S1-3. Heat the solid-liquid mixture obtained in step S1-2 to 60°C, keep it at that temperature for 10 hours, filter to remove residue, and obtain Kanzan cherry blossom water.

2. The use of the composition comprising agarwood extract as described in claim 1 in the preparation of oral hygiene products with antibacterial and bacteriostatic effects.

3. A mouthwash comprising an extract of Aquilaria agallocha, characterized in that, The mouthwash contains the composition comprising agarwood extract as described in claim 1.

4. The mouthwash comprising the extract of Aquilaria crassna according to claim 3, characterized in that, The composition containing agarwood extract is added to the mouthwash in an amount of 4-6 wt%.

5. The mouthwash comprising the extract of Aquilaria crassna according to claim 3, characterized in that, The mouthwash also includes solubilizers, flavoring agents, and solvents.

6. The mouthwash comprising the extract of Aquilaria crassna according to claim 5, characterized in that, The cosolvent is glycerol; The flavoring agent is at least one of acesulfame potassium and menthol; The solvent is deionized water.

7. A method of preparing the mouthwash comprising the extract of Aquilaria crassna according to claim 6, characterized in that, Includes the following steps: S2-1. First, take glycerol, menthol and 1 / 5 of the total amount of deionized water and mix them together. Stir and dissolve them evenly at 100 r / min to obtain mixed solution A. S2-2. Take acesulfame potassium and mix it with 1 / 10 of the total amount of deionized water until it is dissolved evenly to obtain mixed solution B; S2-3. The composition containing agarwood extract, mixed solution A, mixed solution B and the remaining deionized water are mixed and stirred evenly at 200 r / min to obtain the mouthwash containing agarwood extract.

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