Litsea cubeba mouth wash formula and preparation method

Abstract

The invention discloses a litsea cubeba mouthwash formula and a preparation method, and relates to the technical field of mouthwash, and the litsea cubeba mouthwash formula is characterized in that the litsea cubeba mouthwash is composed of the following components by mass volume: 0.05-2% of litsea cubeba essential oil, 0.25-0.35% of citric acid, 1-3% of a sweetener, 0.02-0.06% of menthol, 0.016% of saccharin, 0.5% of Tween-20, and the balance of purified water. The mouth wash prepared by the invention is clear in appearance, fresh in smell and soft and smooth in taste, has a remarkable inhibition effect on staphylococcus aureus and escherichia coli, can effectively clean the oral cavity and improve bad breath, and has relatively high market value.

Description

Technical Field

[0001] The present invention relates to the technical field of mouthwashes, and more specifically, it relates to a formulation and preparation method of a Litsea cubeba mouthwash. Background Art

[0002] With the development of the economic society and the continuous improvement of living standards, people's awareness of oral health care has been greatly enhanced, and oral care products have gradually developed from a single toothpaste to a variety of care products such as toothpaste, dental patches, and mouthwashes. People's consumption purposes have also changed from simple oral cleaning to oral health care and prevention. As an oral health care product, mouthwash is favored by people for its simplicity, convenience, cleanliness and hygiene.

[0003] Litsea cubeba essential oil is a natural essential oil extracted from fresh fruits of Litsea cubeba. It is light yellow in color, and its main chemical components include citral, limonene, methyl heptenone, coriandrol, geraniol, geranial, etc. Litsea cubeba essential oil has good antibacterial, anti-inflammatory, antioxidant and other properties, and is also beneficial for dredging meridians, improving rough and dry skin, and relieving fatigue. It is widely used in the fields of medicine, spices, cosmetics, etc.; however, Litsea cubeba essential oil has a strong pungent smell and taste, which will affect the consumer experience. In view of this, the inventor of the present invention proposes a formulation and preparation method of a Litsea cubeba mouthwash. Summary of the Invention

[0004] The purpose of the present invention is to provide a formulation and preparation method of a Litsea cubeba mouthwash to solve the above problems.

[0005] The above technical purpose of the present invention is achieved through the following technical solutions:

[0006] The first aspect of the present invention provides a formulation and preparation method of a Litsea cubeba mouthwash, which is composed of the following components in mass percentage: Litsea cubeba essential oil 0.05 - 2%, citric acid 0.25 - 0.35%, sweetener 1 - 3%, menthol 0.02 - 0.06%, saccharin 0.016%, Tween - 20 0.5%, and the balance is purified water.

[0007] In combination with the first aspect, the present invention is further set as: Litsea cubeba essential oil 0.05%, citric acid 0.25%, sweetener 1%, menthol 0.02%, saccharin addition amount 0.016%, Tween - 20 0.5%, and the balance is purified water.

[0008] In combination with the first aspect, the present invention is further set as: the sweetener is one or a combination of two of xylitol and sorbitol.

[0009] In combination with the first aspect, the present invention is further set as: the ratio of xylitol to sorbitol is 1:1.

[0010] The second aspect of the present invention also provides a method for preparing a mouthwash, comprising the following steps:

[0011] S1. Weigh Litsea cubeba essential oil and Tween-20 according to the dosages, shake well, slowly add purified water, and stir thoroughly until clear and transparent to obtain a Litsea cubeba-Tween-aqueous solution;

[0012] S2. Add citric acid, sorbitol, xylitol, menthol, and saccharin to the Litsea cubeba-Tween-aqueous solution prepared in step S1 according to the dosages, stir well, and let stand for 2 - 4 h;

[0013] S3. Wait for the solution to cool to room temperature, take the top layer solution to obtain Litsea cubeba essential oil mouthwash

[0014] In combination with the second aspect, the present invention is further configured such that: in step S1, the purified water is at 60 °C.

[0015] In combination with the second aspect, the present invention is further configured such that: in step S1, the mass-volume ratio of Tween-20 to water is 1:200 g / ml.

[0016] In summary, the present invention has the following beneficial effects:

[0017] For the mouthwash prepared by the present invention, through factors such as the addition amount of Litsea cubeba oil, citric acid, sweetening agent, menthol, etc., the preparation formula of Litsea cubeba mouthwash is optimized. Through orthogonal experiments, the optimal formula of Litsea cubeba mouthwash is obtained, that is, the addition amount of Litsea cubeba oil is 0.05%, the addition amount of citric acid is 0.25%, the addition amount of sweetening agent is 1.00%, the addition amount of menthol is 0.02%, the addition amount of saccharin is 0.016%, and the amount of Tween-20 is 0.5%. The mouthwash prepared by the experiment has a clear appearance, a fresh smell, and a smooth taste. This mouthwash shows a significant inhibitory effect on Staphylococcus aureus and Escherichia coli in the antibacterial test, and can effectively clean the oral cavity and improve oral odor, having a high market value. In addition, as a new derivative product of Litsea cubeba oil, this mouthwash provides a strong basis and innovative ideas for the in-depth development and diversified utilization of Litsea cubeba oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is a flowchart of a method for preparing a Litsea cubeba mouthwash in an embodiment of the present invention;

[0019] Figure 2 is the influence of the addition amount of Litsea cubeba essential oil on the sensory evaluation in Test Example 1 of the present invention;

[0020] Figure 3 is the influence of the addition amount of citric acid on the sensory evaluation in Test Example 2 of the present invention;

[0021] Figure 4It is the influence of the addition amount of sweeteners on the sensory evaluation in Test Example 3 of the present invention;

[0022] Figure 5 It is the influence of the addition amount of menthol essential oil on the sensory evaluation in Test Example 4 of the present invention;

[0023] Figure 6 It is the influence of the addition amount of saccharin on the sensory evaluation in Test Example 5 of the present invention;

[0024] Figure 7 It is the orthogonal test result of Litsea cubeba essential oil mouthwash in Test Example 5 of the present invention. Detailed implementation manners

[0025] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0026] Experimental materials

[0027] Litsea cubeba essential oil (self-made in the laboratory); xylitol (batch number 20240920, Shanghai Zhanyun Chemical Co., Ltd.); menthol (batch number 20240801, Shanghai Zhanyun Chemical Co., Ltd.); citric acid (batch number 20240612, Hangzhou Gaojing Fine Chemical Co., Ltd.); D-sorbitol (batch number 20240710, Shanghai Zhanyun Chemical Co., Ltd.); saccharin (batch number 20241202, Shanghai Zhanyun Chemical Co., Ltd.); Tween-20 (batch number 20240215, Shanghai Zhanyun Chemical Co., Ltd.); Wahaha drinking pure water (batch number 202410282223JW4022, Hangzhou Wahaha Group Co., Ltd.); tryptic soy agar medium (TSA medium, batch number 20250109-00, Hangzhou Microbial Reagent Co., Ltd.); gentamicin tablets (batch number 20250225, Hangzhou Microbial Reagent Co., Ltd.); medical physiological saline (batch number XZ9B24040202, Yunnan Tianfei Medical Technology Co., Ltd.); Escherichia coli (Escherichia coli 20250312); Staphylococcus aureus (Staphylococcus aureus 20250312);

[0028] Instruments and equipment

[0029] Electronic analytical balance (model CEB1055N, Shanghai Lichen Bangxi Instrument Technology Co., Ltd.); Electronic balance (model CN-LQC50002, Kunshan Ant Measuring Equipment Co., Ltd.); Digital display constant temperature water bath (model HH-4, Shanghai Lichen Bangxi Instrument Technology Co., Ltd.); Biochemical incubator (model LRH-250, Shanghai Yiheng Scientific Instrument Co., Ltd.); Ultra-clean workbench (model SW-CJ-1D, Shanghai Hujing Medical Instrument Co., Ltd.); Portable high-pressure steam sterilizer (model DSX-24L-1, Shanghai Shen'an Medical Instrument Factory)

[0030] Example 1:

[0031] Weigh 0.25 g of Litsea cubeba essential oil, add 2.5 g of Tween-20, shake well, slowly add 500 mL of pure water at 60 °C, and stir until clear and transparent. Then add 1.0 g of citric acid, 5.0 g of sorbitol, 25.0 g of xylitol, 0.15 g of menthol, and 0.08 g of saccharin, stir well, and let stand for 3 h. After the solution cools to room temperature, take the top 250 mL, fill, sterilize, and label to obtain Litsea cubeba essential oil mouthwash.

[0032] Among them, the preparation method of Litsea cubeba essential oil is to crush the dried Litsea cubeba fruits in a pulverizer, perform steam explosion pretreatment, and then extract Litsea cubeba essential oil by steam distillation method. The extraction rate of the obtained Litsea cubeba essential oil is 6.8%.

[0033] The following experimental examples were evaluated according to Table 1

[0034] Table 1 Characteristic evaluation table of mouthwash

[0035]

[0036]

[0037] Experimental Example 1: Effect of Litsea cubeba essential oil addition amount on the characteristics of mouthwash

[0038] Weigh a certain amount of Litsea cubeba essential oil and prepare Litsea cubeba-Tween-aqueous solutions with contents of 0.05%, 0.1%, 0.15%, 0.2%, 1.5%, and 2% respectively. Prepare Litsea cubeba mouthwash according to the preparation method of Example 1, where the addition amount of Tween-20 is 0.5%, the addition amount of citric acid is 0.2%, the addition amount of sorbitol is 1%, the addition amount of xylitol is 5%, the addition amount of menthol is 0.03%, and the addition amount of saccharin is 0.016%. Let it stand and settle for 3 h, and conduct detection and scoring.

[0039] The effect of Litsea cubeba essential oil addition amount on sensory evaluation is shown in Figure 2。Adding Litsea cubeba essential oil can inhibit the reproduction of oral pathogenic bacteria, reduce the formation of dental plaque, and has a significant effect on bad breath caused by bacteria. However, when the content increases, it will stimulate the oral mucosa and produce a pungent taste. From Figure 2 it can be seen that as the addition amount of Litsea cubeba essential oil increases, the sensory score gradually decreases, and the sensory score is the highest when the addition amount is 0.05%. Therefore, the addition amounts of Litsea cubeba essential oil of 0.05%, 0.15%, and 0.2% are selected as the research levels for the orthogonal experiment.

[0040] Experimental Example 2: Effect of citric acid addition amount on the characteristics of mouthwash

[0041] Weigh a certain amount of citric acid and prepare Litsea cubeba-Tween-aqueous solutions with contents of 0.15%, 0.2%, 0.25%, 0.3%, and 0.35% respectively. Prepare Litsea cubeba mouthwash according to the preparation method of Example 1, where the addition amount of Litsea cubeba essential oil is 0.05%, the addition amount of Tween-20 is 0.5%, the addition amount of sorbitol is 1%, the addition amount of xylitol is 5%, the addition amount of menthol is 0.03%, and the addition amount of saccharin is 0.016%. Let it stand and settle for 3 h, and then conduct detection and scoring.

[0042] The influence of citric acid addition amount on sensory evaluation is shown in Figure 3 。Adding citric acid can not only adjust the taste of the mouthwash, but also eliminate pigmentation and inhibit the growth of dental calculus. From Figure 3 it can be seen that as the addition amount of citric acid increases, the acidity of the product also increases significantly, affecting the overall taste of the mouthwash, and the sensory score gradually increases. The sensory score is the highest when the addition amount is 0.3%. Therefore, the addition amounts of citric acid of 0.25%, 0.3%, and 0.35% are selected as the research levels for the orthogonal experiment.

[0043] Test Example 3: Effect of sweetener addition amount on the characteristics of mouthwash

[0044] Use xylitol and sorbitol in a 1:1 combination as the sweetener. Weigh a certain amount of sorbitol and xylitol and prepare Litsea cubeba-Tween-aqueous solutions with contents of 1%, 2%, 3%, 4%, and 5% respectively. Prepare Litsea cubeba mouthwash according to the preparation method of Example 1, where the addition amount of Litsea cubeba essential oil is 0.05%, the addition amount of Tween-20 is 0.5%, the addition amount of citric acid is 0.2%, the addition amount of xylitol is 5%, the addition amount of menthol is 0.03%, and the addition amount of saccharin is 0.016%. Let it stand and settle for 3 h, and then conduct detection and scoring.

[0045] The influence of sweetener addition amount on sensory evaluation is shown in Figure 4 。Using xylitol and sorbitol in a 1:1 combination as the sweetener enables the product to effectively prevent dental caries while having certain antioxidant properties. After mixing in a 1:1 ratio, the overall sweetness can be adjusted to be closer to sucrose, reducing the high sweetness or blandness of a single sweetener and making the sweetness more natural. FromFigure 4 It can be seen that as the addition amount of the sweetener increases, the sweetness also increases, and the sensory score is the highest when the addition amount is 5%. Therefore, the addition amounts of 1%, 3%, and 5% of the sweetener are selected as the research levels for the orthogonal experiment.

[0046] Experimental Example 4: Influence of the addition amount of menthol on the properties of the mouthwash

[0047] Weigh a certain amount of menthol and prepare Litsea cubeba-Tween-aqueous solutions with the contents of 0.02%, 0.04%, 0.06%, 0.08%, and 0.1% respectively. Prepare Litsea cubeba mouthwash according to the preparation method of Example 1, wherein the addition amount of Litsea cubeba essential oil is 0.05%, the addition amount of Tween-20 is 0.5%, the addition amount of citric acid is 0.2%, the addition amount of sorbitol is 1%, the addition amount of xylitol is 5%, the addition amount of saccharin is 0.016%, let it stand and settle for 3 h, and conduct detection and scoring.

[0048] The influence of the addition amount of menthol on the sensory evaluation is shown in Figure 5 . The addition of menthol will produce a cool mint flavor, which can freshen the breath. If the content is too low, there will be no cool taste, but when the content increases, a certain bitterness will be produced along with a pungent smell. From Figure 5 It can be seen that as the addition amount of menthol increases, the sensory score gradually decreases, and the sensory score is the highest when the addition amount is 0.02%. Therefore, the addition amounts of 0.02%, 0.04%, and 0.06% of menthol are selected as the research levels for the orthogonal experiment.

[0049] Experimental Example 5: Influence of the addition amount of saccharin on the properties of the mouthwash

[0050] Weigh a certain amount of saccharin and prepare Litsea cubeba-Tween-aqueous solutions with the contents of 0.008%, 0.010%, 0.012%, 0.014%, and 0.016% respectively. Prepare Litsea cubeba mouthwash according to the preparation method of Example 1, wherein the addition amount of Litsea cubeba essential oil is 0.05%, the addition amount of Tween-20 is 0.5%, the addition amount of citric acid is 0.2%, the addition amount of sorbitol is 1%, the addition amount of xylitol is 5%, the addition amount of menthol is 0.03%, let it stand and settle for 3 h, and conduct detection and scoring.

[0051] The influence of the addition amount of saccharin on the sensory evaluation is shown in Figure 6 . The addition of saccharin can provide sweetness and improve the taste of the mouthwash, but saccharin should be used within the specified limit, and the addition amount should be strictly controlled. From Figure 5 It can be seen that as the addition amount of saccharin increases, the sensory scores are basically the same, and the sensory score is the highest when the addition amount is 0.016%. Since its influence on the sensory evaluation of the mouthwash is relatively small, the addition amount of saccharin is selected as 0.016%, and the other four factors are selected as the research levels for the orthogonal experiment.

[0052] Experimental Example 6: Orthogonal experiment

[0053] According to the results of the single-factor experiments in Experimental Examples 1 - 4, the four factors that have a greater impact on sensory evaluation, namely Litsea cubeba essential oil, citric acid, sweetener, and menthol, were used as the factors to be investigated, and the addition amounts of other components were fixed: Tween-20 at 0.5% and saccharin at 0.016%. The factor and level design of the orthogonal experiment is shown in Table 2, and the results of the orthogonal experiment are shown in Table 3.

[0054] Table 2 Factor and level table of the orthogonal experiment for Litsea cubeba essential oil mouthwash

[0055]

[0056] Table 3 Results of the orthogonal experiment for Litsea cubeba essential oil mouthwash

[0057]

[0058] As can be seen from Table 3, the highest sensory score was obtained in Test Group 1, namely A1 B1 C1 D1. The results of the range analysis showed that the influence of each factor on sensory evaluation was Litsea cubeba essential oil > citric acid > menthol > sweetener, and the best combination was A1 B1 C1 D1. Verification tests were carried out according to this condition, and three parallel tests were conducted respectively. The results were 89, 91, and 92, with an average of 90.7 points. Therefore, the optimal formula for the mouthwash was determined as follows: the addition amount of Litsea cubeba essential oil was 0.05%, the addition amount of citric acid was 0.25%, the addition amount of sweetener was 1%, and the addition amount of menthol was 0.02%. The addition amounts of Litsea cubeba essential oil, citric acid, sweetener, and menthol at different levels all had significant effects on the sensory score of the mouthwash, and the addition amount of Litsea cubeba essential oil had the greatest influence.

[0059] Experimental Example 7: Antibacterial test

[0060] Based on the above orthogonal experiment, the formula with the best taste was used to continue the antibacterial tests against Escherichia coli and Staphylococcus aureus.

[0061] Table 4 Antibacterial test results of Litsea cubeba essential oil mouthwash

[0062]

[0063] As can be seen from Table 4, Litsea cubeba mouthwash had antibacterial effects against two common pathogenic bacteria. The antibacterial rate against Escherichia coli was 62.6%, and the antibacterial rate against Staphylococcus aureus was 64.9%. Thus, it can be seen that the Litsea cubeba essential oil mouthwash prepared according to the optimal formula had antibacterial effects, could effectively clean the oral cavity and freshen the breath, and this result provided a theoretical basis for the development of natural antibacterial oral care products based on Litsea cubeba essential oil. Compared with the common chemical mouthwashes that generally had an antibacterial rate of over 60% against these two strains, although there was a certain gap, the Litsea cubeba essential oil mouthwash had unique advantages in the ecological friendliness of its natural ingredients.

[0064] Finally, it should be noted that the above are only 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 perform equivalent replacements for some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A Litsea cubeba mouthwash formula, characterized in that: The invention is composed of the following components in mass volume percentage: 0.05-2% of Litsea cubeba essential oil, 0.25-0.35% of citric acid, 1-3% of sweetener, 0.02-0.06% of menthol, 0.016% of saccharin, 0.5% of Tween-20, and the balance of water.

2. A Litsea cubeba mouthwash formula according to claim 1, characterized in that: 0.05% of Litsea cubeba essential oil, 0.25% of citric acid, 1% of sweetener, 0.02% of menthol, 0.016% of saccharin addition, 0.5% of Tween-20, and the balance of water.

3. A Litsea cubeba mouthwash formula according to claim 1 or 2, characterized in that: The sweetener is one or a combination of xylitol and sorbitol.

4. A Litsea cubeba mouthwash formula according to claim 3, characterized in that: The ratio of xylitol to sorbitol is 1:

1.

5. The method for preparing the mouthwash according to any one of claims 1 to 4, characterized in that: The steps include: S1. Weigh the essential oil and Tween-20 according to the amount, shake well to mix, slowly add water, stir until clear and transparent, and obtain a Litsea cubeba-Tween-water solution; S2. Add citric acid, sorbitol, xylitol, menthol and saccharin to the litsea cubeba-Tween-water solution prepared in step S1, stir well and let stand for 2-4h; S3. After the solution is cooled to room temperature, take the supernatant to obtain the Litsea cubeba essential oil mouthwash.

6. The method for preparing the mouthwash according to claim 5, characterized in that: In step S1, the water is 60°C pure water.

7. The method for preparing the mouthwash according to claim 5, characterized in that: In step S1, the mass volume ratio of Tween-20 to water is 1:200 g / ml.

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