Antibacterial composition, product and preparation method

Abstract

The invention belongs to the field of traditional Chinese medicines, and particularly relates to a bacteriostatic composition, a product and a preparation method. The bacteriostatic composition provided by the invention comprises the following bacteriostatic active components: elsholtzia volatile oil, eupatorium volatile oil, honeysuckle extract and humifuse euphorbia herb extract, and the weight ratio of the elsholtzia volatile oil to the eupatorium volatile oil to the honeysuckle extract to the humifuse euphorbia herb extract in the bacteriostatic active components is (0.5-2): (0.2-1): (1-4): (1-4). The bacteriostatic composition and the toothpaste product containing the bacteriostatic composition provided by the invention have a remarkable inhibition effect on the activity of escherichia coli and staphylococcus aureus, and when the addition amount of the toothpaste is 50 mu L, the diameter of an inhibition zone on the escherichia coli reaches 3.25 cm, and the diameter of an inhibition zone on the staphylococcus aureus reaches 1.62 cm.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine, specifically relating to an antibacterial composition, product, and preparation method. Background Technology

[0002] The balance of the oral microecology is crucial for maintaining oral health, while the overgrowth of microorganisms such as bacteria and fungi is the main cause of oral problems such as tooth decay, gingivitis, periodontitis, and halitosis.

[0003] In recent years, with increasing attention to oral health, more and more oral care products have begun to use natural Chinese herbal ingredients to replace chemical antibacterial agents. Furthermore, since the effects of a single Chinese herbal ingredient are extremely limited, most oral antibacterial products combine multiple Chinese herbs, such as patents CN108721180A, CN102038781A, and CN101933977A.

[0004] Although toothpaste containing traditional Chinese medicine ingredients has the advantage of being natural and safe, there are many types of traditional Chinese medicinal herbs, and the types and structures of their active ingredients vary significantly. Therefore, the antibacterial effect of different types of Chinese medicinal herbs may vary greatly when they are combined. In pursuit of "multi-effect", most products blindly combine multiple Chinese medicinal herbs without considering the interactions between the ingredients, which can easily lead to unreasonable ingredient combinations. For example, patent CN1368206A adds honeysuckle, coptis, and gardenia at the same time. Some alkaloids in coptis (such as berberine) may form precipitates in aqueous solution with flavonoids in honeysuckle and gardenia (such as rutin), reducing the bioavailability of each Chinese medicinal herb. In addition, some Chinese medicinal herbs can irritate the oral mucosa when the concentration is too high, and have no antibacterial effect when the concentration is too low. Existing products have difficulty in accurately controlling the ratio.

[0005] Therefore, developing a traditional Chinese medicine antibacterial agent composition with clearly defined ingredients, scientific compatibility, and significant antibacterial effect has become an important research direction in the field of oral care. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides an antibacterial composition, product, and preparation method.

[0007] The first aspect of the present invention is to provide an antibacterial composition, wherein the antibacterial active ingredient of the antibacterial composition provided by the present invention is composed of Elsholtzia volatile oil, Eupatorium fortunei volatile oil, Lonicera japonica extract, and Euphorbia humifusa extract, wherein the weight ratio of Elsholtzia volatile oil: Eupatorium fortunei volatile oil: Lonicera japonica extract: Euphorbia humifusa extract is 0.5-2:0.2-1:1-4:1-4.

[0008] Preferably, the antibacterial active ingredients of the antibacterial composition have a weight ratio of Elsholtzia volatile oil: Eupatorium fortunei volatile oil: Lonicera japonica extract: Euphorbia humifusa extract of 1.5:0.8:2:4.

[0009] Elsholtzia ciliata, the dried aerial parts of the Lamiaceae plant Elsholtzia ciliata or Elsholtzia jiangnanensis, is rich in volatile oils. These volatile oils mainly contain various active ingredients such as elsholtzone, acetophenone, β-sitosterol, palmitic acid, linoleic acid, linolenic acid, and ursolic acid. Elsholtzia ciliata is slightly warm in nature and pungent in taste, and has the effects of inducing sweating and relieving exterior syndromes, promoting diuresis and reducing swelling, and harmonizing the stomach and resolving dampness.

[0010] Eupatorium fortunei, a perennial herb belonging to the genus Eupatorium in the family Asteraceae, is described in the *Shennong Bencao Jing* as having the properties of "pungent, neutral, promoting urination, killing poisons, dispelling misfortune, invigorating qi, and enhancing mental clarity; it is also known as 'Water Fragrance'." Studies have shown that the whole plant contains 1.5%-2.0% volatile oil, which includes p-cymene, nerol ethyl ester, 5-methylthymol, fumaric acid, succinic acid, mannitol, etc. The leaves contain o-coumaric acid, coumarin, and thymol hydroquinone. The flowers contain taraxasterol, taraxasterol palmitate, taraxasterol acetate, etc. The aerial parts and roots contain dipyrrolidine alkaloids, including heliotropin, ningdrolofine, and styracin.

[0011] Honeysuckle, the dried flower buds or newly opened flowers of the honeysuckle plant (Lonicera japonica), is rich in volatile oils, flavonoids, organic acids, and triterpenoid saponins. Among them, the flavonoids are mainly luteolin, and the organic acids are mainly chlorogenic acid and isochlorogenic acid, as well as myristic acid, palmitic acid, caffeic acid, protocatechuic acid, etc. It has antibacterial, antiviral, anti-inflammatory, antireplicative and antioxidant effects.

[0012] Euphorbia humifusa, the dried whole herb of Euphorbia humifusa in the Euphorbiaceae family, mainly contains flavonoids (such as quercetin and its glycosides, kaempferol and its glycosides), terpenoids (such as sesquiterpenes and triterpenoids), and phenolic compounds (tannins), exhibiting a variety of biological activities such as antioxidation, anti-inflammation, antibacterial, antiviral, immunomodulatory, hepatoprotective, and hemostatic effects.

[0013] During their research, the inventors discovered that single Chinese herbal ingredients had extremely poor antibacterial effects when used as antibacterial agents. Therefore, they combined two Chinese herbal ingredients. However, the antibacterial effects of the combinations obtained by combining the two ingredients were completely different. For example, for Escherichia coli, the combination of honeysuckle and agastache showed the best antibacterial effect, while the combination of honeysuckle and euphorbia humifusa had a very poor antibacterial effect. In addition, for Staphylococcus aureus, the combination of agastache with elsholtzia ciliata or honeysuckle had a much better antibacterial effect than the combination of honeysuckle and euphorbia humifusa.

[0014] When the inventors combined the above-mentioned traditional Chinese medicine ingredients, and adjusted the preparation process of the active ingredients in each traditional Chinese medicine ingredient and the addition ratio of each ingredient, they obtained an antibacterial composition with the best antibacterial effect.

[0015] A second aspect of the present invention is that a method for preparing the above-mentioned antibacterial composition is provided, specifically a method for preparing various antibacterial active ingredients in the antibacterial composition. Specifically, the methods for preparing the various antibacterial active ingredients are as follows: Elsholtzia / Eupatorium fortunei volatile oil: Take the aerial parts of Elsholtzia / Eupatorium fortunei, dry them and pulverize them into Elsholtzia / Eupatorium fortunei powder. Add water at a mass-volume ratio of 1g: 8-10mL and use ultrasonic-assisted extraction. First, extract at 20-35℃ for 20-40 min, and then distill in boiling water for 1-2 h to obtain Elsholtzia / Eupatorium fortunei volatile oil.

[0016] Honeysuckle extract: After pulverizing honeysuckle, add 60%-80% ethanol at a mass-to-volume ratio of 1 g: 8-15 mL. Use ultrasound-assisted extraction at 30-50 ℃ for 20-60 min, and then reflux at 60-80 ℃ for 2-3 times, each time for 1-2 h. After filtration, concentrate the extract under reduced pressure and dry to obtain honeysuckle extract.

[0017] Euphorbia humifusa extract: After drying and pulverizing Euphorbia humifusa, add 60%-80% ethanol at a mass-to-volume ratio of 1 g: 8-15 mL, and reflux extract at 60-90 ℃ for 2-3 times, 1.5-3 h each time. After filtering the extract, concentrate under reduced pressure to make an extract, dry it, and obtain Euphorbia humifusa extract.

[0018] As a preferred embodiment, the preparation method of the Elsholtzia volatile oil is as follows: Elsholtzia var. ...

[0019] As a preferred method, the preparation method of the Eupatorium fortunei volatile oil is as follows: Eupatorium fortunei is dried and pulverized into Eupatorium fortunei powder. Water is added at a mass-volume ratio of 1g:10mL, and ultrasonic-assisted extraction is performed. First, it is extracted at 30℃ for 30 min, then steam distilled at 100℃ for 2 h, and dehydrated with anhydrous sodium sulfate for 1 h to obtain Eupatorium fortunei volatile oil.

[0020] As a preferred embodiment, the honeysuckle extract is prepared by: pulverizing honeysuckle, adding 70% ethanol at a mass-to-volume ratio of 1 g: 10 mL, using ultrasonic-assisted extraction at 40 ℃ for 30 min, and then refluxing at 70 ℃ twice for 1.5 h each time. After filtration, the extract is concentrated under reduced pressure and dried to obtain the honeysuckle extract.

[0021] As a preferred embodiment, the preparation method of the *Euphorbia humifusa* extract is as follows: after drying and pulverizing *Euphorbia humifusa*, 70% ethanol is added at a mass-volume ratio of 1 g: 10 mL, and the mixture is refluxed at 80°C twice for 2 hours each time. After filtering the extract, it is concentrated under reduced pressure to prepare an extract, which is then dried to obtain the *Euphorbia humifusa* extract.

[0022] Preferably, during the preparation of the above-mentioned antibacterial components, the ultrasonic frequency during ultrasonic-assisted extraction is 30-50 kHz.

[0023] As a further preferred embodiment, the frequency of the ultrasound during the ultrasound-assisted extraction is 35-45 kHz.

[0024] A third aspect of the present invention is that a product containing the above-described antibacterial composition is provided, the product including toothpaste, mouthwash, and chewing gum, wherein the dosage form of the mouthwash includes, but is not limited to, liquid, solid tablets, and popping beads.

[0025] A fourth aspect of the present invention is to provide a toothpaste containing the above-mentioned antibacterial composition, comprising, by weight, 5-10 parts of the antibacterial composition, 38-45 parts of an abrasive, 15-25 parts of a humectant, 0.8-1.5 parts of a thickener, 1.2-1.8 parts of a foaming agent, and 20-35 parts of water.

[0026] Preferably, the toothpaste comprises, by weight, 8.3 parts of an antibacterial composition, 40 parts of an abrasive, 20 parts of a humectant, 1.2 parts of a thickener, 1.5 parts of a foaming agent, and 29 parts of water.

[0027] The beneficial effects of this invention are as follows: This invention uses Elsholtzia volatile oil, Eupatorium fortunei volatile oil, honeysuckle extract, and Euphorbia humifusa extract as the antibacterial active ingredients in an antibacterial composition. By adjusting the preparation process and proportions of the above ingredients, the resulting antibacterial composition exhibits significant antibacterial activity when used in toothpaste. When the toothpaste addition amount is 50 μL, the inhibition zone diameter against Escherichia coli reaches 3.25 cm, and the inhibition zone diameter against Staphylococcus aureus reaches 1.62 cm. Attached Figure Description

[0028] Figure 1 The diagram shows the antibacterial test results of the toothpaste prepared in this invention against Escherichia coli and Staphylococcus aureus. Figure 2 The graph shows the effect of the amount of abrasives, humectants, thickeners, and foaming agents added to toothpaste on the sensory score of toothpaste. Figure 3 Contour plots and response surface plots showing the relationship between the amounts of abrasives, humectants, and thickeners added in toothpaste. Detailed Implementation

[0029] To enable those skilled in the art to better understand the present invention, the present invention will now be further described in conjunction with specific embodiments.

[0030] Example 1 A toothpaste containing an antibacterial composition, wherein the toothpaste comprises 40 parts of an abrasive, 20 parts of a humectant, 1.2 parts of a thickener, 1.5 parts of a foaming agent, 8.3 parts of the antibacterial composition, and 29 parts of water.

[0031] The antibacterial composition consists of four antibacterial active ingredients: Elsholtzia volatile oil, Eupatorium fortunei volatile oil, honeysuckle extract, and Euphorbia humifusa extract.

[0032] The preparation methods of each antibacterial active ingredient in the antibacterial composition are as follows: Eupatorium fortunei volatile oil: After the raw material of Eupatorium fortunei was air-dried and pulverized for pretreatment, water was added at a mass-volume ratio of 1 g: 10 mL. The mixture was first extracted with ultrasound assistance at 30 ℃ for 30 min, and then steam distilled at 100 ℃ for 2 h. After the distillation product was cooled, it was dehydrated with anhydrous sodium sulfate for 1 h to obtain the volatile oil of Eupatorium fortunei. The frequency of ultrasound during the extraction process was 40 kHz.

[0033] Elsholtzia volatile oil: The raw material of Elsholtzia var. ...

[0034] Honeysuckle extract: After pulverizing honeysuckle, it was extracted by ultrasonic immersion in 70% ethanol at a material-liquid ratio of 1 g: 10 mL at 40 ℃ for 30 min, followed by two reflux extractions at 70 ℃ for 1.5 h each time. The extract was filtered, concentrated under reduced pressure (temperature ≤ 50 ℃), and then dried in an oven to obtain honeysuckle extract.

[0035] Euphorbia humifusa extract: After drying and pulverizing Euphorbia humifusa, it was extracted twice by reflux at 80 °C for 2 h each time using 70% ethanol as solvent at a mass-volume ratio of 1 g: 10 mL. The extract was filtered, concentrated under reduced pressure to prepare an extract, and then freeze-dried to obtain Euphorbia humifusa extract.

[0036] Using refreshing sensation, bitterness, sweetness, aroma, and color as scoring criteria, 10 volunteers were invited to conduct sensory evaluations of the toothpaste prepared in this embodiment. The difference between the toothpastes lies in the different proportions of antibacterial active ingredients in the antibacterial composition added to each toothpaste.

[0037] The evaluation criteria for the sensory evaluation form are shown in Table 1 below, and the sensory scores of toothpastes with different antibacterial compositions are shown in Table 2 below.

[0038] Table 1 Sensory Evaluation Criteria index Scoring details (18-20 points) Scoring details (14-17 points) Scoring details (0-13 points) Refreshing The cooling sensation is long-lasting and non-irritating. The cooling sensation is moderate, with a slight irritation. No cooling sensation, noticeably irritating. bitterness No bitterness, smooth taste Slightly bitter, but acceptable. It is distinctly bitter and difficult to accept. Sweetness The sweetness is just right, and it tastes natural. Too sweet or not sweet enough Abnormal or absent sweetness fragrance Harmony of medicinal fragrance and perfume The fragrance is slightly strong or mild. The fragrance is pungent or the odor is obvious. Color Light brown color, even texture, good gloss Slightly darker or slightly uneven in color Dull color or obvious layering

[0039] Table 2 Sensory ratings of toothpastes with different antibacterial compositions experimental group Perrin volatile oil Elsholtzia volatile oil Honeysuckle extract Euphorbia humifusa extract Sensory rating 1 0.2 0.5 1 1 82.5 2 0.2 1 2 2 84.2 3 0.2 1.5 3 3 89.2 4 0.2 2 4 4 97.8 5 0.4 0.5 2 3 86.2 6 0.4 1 1 4 88.5 7 0.4 1.5 4 1 94.2 8 0.4 2 3 2 92.5 9 0.6 0.5 3 4 85.5 10 0.6 1 4 3 95.5 11 0.6 1.5 1 2 87.8 12 0.6 2 2 1 91.8 13 0.8 0.5 4 2 93.8 14 0.8 1 3 1 80.8 15 0.8 1.5 2 4 97.8 16 0.8 2 1 3 90.5

[0040] The results in Table 2 show that the ratio of antibacterial active ingredients in the antibacterial composition has a significant impact on the sensory properties of toothpaste after adding the antibacterial composition. Due to the strong odor of Eupatorium fortunei volatile oil, toothpaste exhibits a noticeable irritating taste when the content of Eupatorium fortunei volatile oil is too high; the color is unappealing when the content of Elsholtzia ciliata volatile oil is too high; the irritating taste is obvious when the content of Lonicera japonica extract is too high; and the bitter taste is too obvious when the content of Euphorbia humifusa extract is too high. Therefore, as can be seen from the table, the toothpaste with the antibacterial composition of group 15 showed the best sensory score, followed by group 4 and group 10.

[0041] Example 2 The toothpastes in groups 4, 10, and 15 prepared in Example 1 were used for antibacterial activity tests to verify their antibacterial effects on Escherichia coli and Staphylococcus aureus. The antibacterial effects of toothpastes with different antibacterial compositions on Escherichia coli and Staphylococcus aureus are shown in Table 3 below.

[0042] Table 3. Antibacterial effects of different types and dosages of toothpaste

[0043] Table 3 shows that for Escherichia coli and Staphylococcus aureus, the antibacterial effect generally increased with the increase of toothpaste dosage. However, when the toothpaste dosage was 75 μL, there was no significant difference in antibacterial activity compared to 50 μL. Therefore, in order to save costs, the amount of toothpaste used should be 50 μL.

[0044] Meanwhile, Table 3 also shows that although the sensory scores of the toothpastes in groups 4, 10, and 15 of the experimental group were not significantly different, and their palatability and acceptability were relatively high, the antibacterial effects of the three groups of toothpastes were significantly different. In particular, when the amount of toothpaste added was 50 μL, the inhibition zone of group 15 toothpaste against Escherichia coli was 3.25 cm, which was much higher than the 1.8 cm of group 4 and the 2.4 cm of group 10, showing the best antibacterial effect.

[0045] Figure 1 The graph shows the inhibitory effects of toothpaste groups 4, 10, and 15 on Escherichia coli (A) and Staphylococcus aureus (B) when the toothpaste addition amount is 50 μL. It can be clearly seen from the graph that the antibacterial effect of toothpaste group 15 is the most significant.

[0046] Comparative Example 1 The toothpaste prepared in this comparative example contains 40 parts of abrasive, 20 parts of humectant, 1.2 parts of thickener, 1.5 parts of foaming agent, 4 parts of antibacterial composition, and 29 parts of distilled water. The weight parts of each component in the antibacterial composition are shown in Table 4 below.

[0047] The antibacterial effects of different toothpastes were verified using the same method as in Example 2, with 50 μL of toothpaste used in each case. The experimental results are shown in Table 4 below.

[0048] Table 4. Antibacterial effects of toothpastes with different antibacterial compositions

[0049] All components listed in Table 4 are weight percentages.

[0050] Table 4 shows that when antibacterial ingredients are combined in pairs as an antibacterial composition, the antibacterial effect of toothpaste is significantly reduced. Specifically, against *Escherichia coli*, the combination of *Eupatorium fortunei* and honeysuckle had the largest inhibition zone diameter, only 1.60 cm, indicating a significant synergistic effect. The combination of honeysuckle and *Euphorbia humifusa* had the smallest inhibition zone diameter, 1.17 cm, indicating a weaker synergistic effect. For *Staphylococcus aureus*, the combination of *Eupatorium fortunei* and *Elsholtzia ciliata* had the largest inhibition zone diameter, 1.52 cm, showing a significant synergistic effect, while the combination of *Elsholtzia ciliata* and *Euphorbia humifusa* had the smallest inhibition zone diameter, 1.35 cm, indicating a relatively weaker synergistic effect.

[0051] Comparative Example 2 Unlike Example 1, the toothpaste prepared without the addition of an antibacterial composition has no antibacterial activity.

[0052] Based on this, the effects of the amount of abrasives, humectants, thickeners, foaming agents, and other components added to the toothpaste base on the toothpaste's forming, stability, paste form, foam volume, and other performance parameters were investigated. Ten volunteers were invited to conduct sensory evaluations, and the standards for sensory evaluation are shown in Table 5 below.

[0053] Table 5 Sensory Evaluation Criteria project Scoring details (81-100 points) Scoring details (61-80 points) Scoring details (0-60 points) Forming status The fibers are clearly visible and there is no collapse. The surface is slightly brittle and has a slight collapse. No wire drawing, severe collapse ointment form Fine and even texture, with a glossy color Slightly grainy texture, slightly dark color Noticeable particles, uneven color stability No layering Slight stratification Severe separation, liquefaction of the ointment Foam volume The amount of foam was the same as that of the reference standard. Too much or too little foam No foam

[0054] The specific procedures for the experiment on the effects of each ingredient on the sensory evaluation of toothpaste are as follows: The effect of the amount of abrasive added on the sensory score of toothpaste: 20 parts of humectant, 1.2 parts of thickener, 1.5 parts of foaming agent, and 30, 35, 40, 45 and 50 parts of abrasive respectively.

[0055] The effect of the amount of humectant added on the sensory score of toothpaste: 40 parts of abrasive, 1.2 parts of thickener, 1.5 parts of foaming agent, and 10, 15, 20, 25 and 30 parts of humectant respectively.

[0056] The effect of thickener addition on the sensory score of toothpaste: 40 parts abrasive, 20 parts humectant, 1.5 parts foaming agent, and 0.4 parts, 0.8 parts, 1.2 parts, 1.6 parts, and 2.0 parts thickener, respectively.

[0057] The effect of foaming agent addition on the sensory score of toothpaste: 40 parts abrasive, 20 parts humectant, 1.2 parts thickener, and 0.5 parts, 1.0 parts, 1.5 parts, 2.0 parts, and 2.5 parts foaming agent, respectively.

[0058] The sensory evaluation results of each toothpaste ingredient are shown below. Figure 2 As shown.

[0059] Figure 2 It can be seen that the sensory score of toothpaste generally shows a trend of first increasing and then decreasing as the amount of abrasive, humectant, thickener and foaming agent added increases. When the amount of abrasive added is 40 parts, the amount of humectant added is 20 parts, the amount of thickener added is 1.2 parts, and the amount of foaming agent added is 1.5 parts, the sensory score of toothpaste is the highest under the same conditions.

[0060] A Box-Behnken design was adopted, with sensory evaluation values ​​as the response values. The amount of abrasive added (A), humectant added (B), and thickener added (C) were used as three factors to conduct a response surface design, as shown in Table 6. The results of the response surface design experiment and sensory scoring are shown in Table 7.

[0061] Table 6. Response Surface Design of Toothpaste Matrix (n=3) level A（%） B（%） C（%） -1 35 15 0.8 0 40 20 1.2 1 45 25 1.6

[0062] Table 7 Response Surface Design Experiments and Sensory Scoring Test No. A B C Sensory rating 1 -1 -1 0 65.18 2 1 -1 0 70.00 3 -1 1 0 68.73 4 1 1 0 69.55 5 -1 0 -1 71.82 6 1 0 -1 76.18 7 -1 0 1 76.82 8 1 0 1 78.27 9 0 -1 -1 80.10 10 0 1 -1 81.82 11 0 -1 1 83.09 12 0 1 1 84.64 13 0 0 0 90.00 14 0 0 0 90.09 15 0 0 0 90.27 16 0 0 0 90.55 17 0 0 0 90.82

[0063] Using Design-Expert 13 software, multiple linear regression and quadratic multinomial fitting were performed on the data shown in Table 7. The regression equation between the sensory evaluation value of the toothpaste matrix and each factor was obtained as follows: Y = 90.346 + 1.43125A - 0.7525B + 1.56875C - 1AB - 0.7275AC + 0.045BC - 14.3543A 2 -7.62675B 2 -0.21925C 2 .

[0064] As shown in Table 8, this regression model P <0.01, lack of fit term >0.05, indicating the model is highly significant and statistically significant, R0.05 2 =0.9993, which is greater than 0.9, indicates that the equation has a high good fit and good predictive ability. The F-value shows that the influence of the three factors on the sensory score of the toothpaste matrix is: A > C > B, i.e., abrasive > thickener > humectant.

[0065] Table 8. Analysis of Variance Table Source of mutation sum of squares Degrees of freedom Mean Square F value value Significance Model 1219.74 9 135.53 1190.18 <0.0001 ** A 16.39 1 16.39 143.92 <0.0001 ** B 4.53 1 4.53 39.78 0.0004 ** C 19.69 1 19.69 172.9 <0.0001 ** AB 4 1 4 35.13 0.0006 ** AC 2.12 1 2.12 18.59 0.0035 * BC 0.0081 1 0.0081 0.0711 0.7974 A2 867.56 1 867.56 7618.78 <0.0001 ** B2 244.92 1 244.92 2150.82 <0.0001 ** C2 0.2024 1 0.2024 1.78 0.2242 residual 0.7971 7 0.1139 Missing item 0.0339 3 0.1133 0.9906 0.4822 Pure error 0.4573 4 0.1143 comprehensive 1220.53 16

[0066] Note: If P > F, then there is no significance. ** indicates highly significant, * indicates significant.

[0067] Using Design-expert 13 software, contour plots and response surface plots were generated for the three components: abrasive (A), humectant (B), and thickener (C). The results are shown in [Figure number missing]. Figure 3 .

[0068] Figure 3 The response surfaces of (A) and (C) are steep, the contour plots are nearly elliptical, and the color changes are obvious, indicating that the two interactions are strong and have a significant impact on the sensory score of the toothpaste matrix; the response surface curve of (E) is relatively flat, indicating that the interaction between the humectant and the thickener has a significant impact on the toothpaste matrix.

Claims

1. An antibacterial composition, characterized in that, The antibacterial active ingredients of the antibacterial composition are composed of Elsholtzia volatile oil, Eupatorium fortunei volatile oil, Lonicera japonica extract, and Euphorbia humifusa extract. The weight ratio of Elsholtzia volatile oil: Eupatorium fortunei volatile oil: Lonicera japonica extract: Euphorbia humifusa extract is 0.5-2:0.2-1:1-4:1-4.

2. The antibacterial composition according to claim 1, characterized in that, The weight ratio of the antibacterial active ingredients, namely, Elsholtzia zedoaria volatile oil, Eupatorium fortunei volatile oil, Lonicera japonica extract, and Euphorbia humifusa extract, is 1.5:0.8:2:

4.

3. The antibacterial composition according to any one of claims 1-2, characterized in that, In the aforementioned antibacterial composition, each antibacterial active ingredient is prepared using the following methods: Elsholtzia / Eupatorium fortunei volatile oil: Take the aerial parts of Elsholtzia / Eupatorium fortunei, dry them and pulverize them into Elsholtzia / Eupatorium fortunei powder. Add water at a mass-volume ratio of 1 g: 8-10 mL. First, extract with ultrasonic assistance at 20-35 ℃ for 20-40 min, and then distill in boiling water for 1-2 h to obtain Elsholtzia / Eupatorium fortunei volatile oil. Honeysuckle extract: After pulverizing honeysuckle, add 60%-80% ethanol at a mass-volume ratio of 1 g: 8-15 mL, and extract with ultrasonic assistance at 30-50 ℃ for 20-60 min. Then, reflux extract at 60-80 ℃ for 2-3 times, 1-2 h each time. After filtering the extract, concentrate under reduced pressure and dry to obtain honeysuckle extract. Euphorbia humifusa extract: After drying and pulverizing Euphorbia humifusa, add 60%-80% ethanol at a mass-to-volume ratio of 1 g: 8-15 mL, and reflux extract at 60-90 ℃ for 2-3 times, 1.5-3 h each time. After filtering the extract, concentrate under reduced pressure to make an extract, dry it, and obtain Euphorbia humifusa extract.

4. The antibacterial composition according to claim 3, characterized in that, During ultrasound-assisted extraction, the frequency of the ultrasound is 30-50kHz.

5. A product containing the antibacterial composition of claim 1, characterized in that, This includes toothpaste, mouthwash, and chewing gum, with the mouthwash dosage forms including, but not limited to, liquid, solid lozenges, and popping beads.

6. A toothpaste containing the antibacterial composition of claim 1, characterized in that, By weight, it comprises 5-10 parts of antibacterial composition, 38-45 parts of abrasive, 15-25 parts of humectant, 0.8-1.5 parts of thickener, 1.2-1.8 parts of foaming agent, and 20-35 parts of water.

7. The toothpaste as described in claim 6, characterized in that, The composition comprises, by weight, 8.3 parts of antibacterial composition, 40 parts of abrasive, 20 parts of humectant, 1.2 parts of thickener, 1.5 parts of foaming agent, and 29 parts of water.

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