A dental caries-preventing oral care composition containing Patchouli alcohol and its application

Abstract

The present invention discloses a dental caries-preventing oral care composition containing Patchouli alcohol and its application. The composition comprises component A, component B and component C, wherein component A is Patchouli alcohol, component B is at least one of magnolol and bornyl acetate, and component C comprises at least one of citral, ethyl p-methoxycinnamate or β-caryophyllene; wherein the contents of component A and component B are greater than zero, and the content of component C is greater than or equal to zero. The scheme of the present invention innovatively proposes to scientifically proportion Patchouli alcohol with one or more of the natural active ingredients such as magnolol and bornyl acetate to form an efficient antibacterial and dental caries-preventing composition. The composition can be widely used in various oral care products, including but not limited to toothpaste, tooth powder, liquid toothpaste, mouthwash, tooth paste, chewing gum, oral spray and tooth gel, etc., aiming to provide users with all-round and multi-level oral health protection.

Description

Technical Field

[0001] The invention relates to the technical field of oral care, and in particular to an anti-caries oral care composition containing patchouli alcohol and an application thereof. Background Art

[0002] Dental caries, commonly known as tooth decay or tooth decay, is a common and frequently occurring oral disease. Dental caries is a bacterial disease, so it can cause pulpitis, jaw inflammation, etc. Secondary infection of dental caries can form lesions, causing or adding to other systemic diseases such as arthritis, pericarditis, chronic nephritis, etc. It is estimated that the total number of cases of oral diseases worldwide is 1 billion more than the total number of cases of all five major non-communicable diseases (mental disorders, cardiovascular diseases, diabetes, chronic respiratory diseases and cancer). Dental caries is a bacterial biofilm disease caused by multiple factors. Repeated stimulation of bacterial acid production leads to mineral loss and destruction of tooth structure. The imbalance of oral microbial community homeostasis is a key factor leading to the occurrence of dental caries. After bacteria adhere to the surface of teeth to form dental plaque, they ferment and produce acid at a suitable temperature to destroy tooth enamel and form dental caries. Streptococcus mutans is the main cariogenic bacteria. Streptococcus mutans can cause acidification of the oral microenvironment, adapt to the slightly acidic oral environment, and inhibit the activity of other symbiotic bacteria in the oral microecological system. It can use extracellular glycosyltransferase to synthesize extracellular polysaccharides with sucrose as a substrate to promote the formation of tooth surface ecological film and participate in the composition of tooth surface ecological film matrix. At the same time, Streptococcus mutans has a high affinity for hydroxyapatite on the tooth surface, and its adhesion to the tooth surface gives it a unique ability to cause smooth surface caries, while other bacteria rarely cause smooth surface caries.

[0003] At present, fluoride and antibiotic treatment have been proven to have a good effect in preventing dental caries and can effectively inhibit cariogenic bacteria in the oral cavity, but they have certain limitations and side effects. Long-term use of antibiotics can easily cause dysbiosis of oral flora and easily develop drug resistance. Excessive fluoride can cause chronic fluorosis and dental fluorosis (usually in children under 6 years old). Excessive fluoride is combined with developing teeth, leading to poor tooth development. In addition, the use of fluoride should be determined according to the fluoride content in the body, the fluoride content in drinking water, etc., so the application of fluoride in dental caries is limited. Natural products are rich in sources, have few side effects and significant efficacy, so in recent years, the application of natural medicines in dental caries prevention has gradually become a research hotspot in the field of oral health.

[0004] Patchouli alcohol is the main component of the patchouli plant Pogostemon cablin (Blanco) Benth. of the Lamiaceae family. It is an important indicator for evaluating the quality of patchouli and its essential oil in the Chinese Pharmacopoeia, and is also considered to be the main contributing component to the pharmacological efficacy and fragrance of patchouli essential oil. The pharmacological effects of Patchouli alcohol have gradually become a research hotspot. It has anti-influenza virus, anti-depression, anti-vascular relaxation, lung protection, brain protection, anti-ulcer, anti-colitis, prebiotic-like, anti-inflammatory, anti-cancer and protective activities against metabolic diseases. Patchouli alcohol has always attracted much attention in the antibacterial and anti-fungal and anti-pathogenic microorganisms, and has good therapeutic effects in the treatment of Helicobacter pylori, Candida albicans and other infections. However, to date, there has been no research and application of Patchouli alcohol in the field of oral care such as dental caries caused by bacterial diseases, and in oral care products for dental caries prevention. Summary of the invention

[0005] The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the present invention provides an anti-caries composition containing Patchouli alcohol, which can resist the formation of dental plaque and caries for a long time while having antibacterial and anti-inflammatory effects.

[0006] The present invention also provides the application of the composition.

[0007] The anti-caries oral care composition according to the first aspect of the embodiment of the present invention comprises component A, component B and component C, wherein component A is patchouli alcohol, component B is at least one of magnolol and borneol acetate, and component C comprises at least one of citral, ethyl p-methoxycinnamate or β-caryophyllene; wherein the contents of component A and component B are greater than zero, and the content of component C is greater than or equal to zero.

[0008] The anti-caries oral care composition according to the embodiment of the present invention has at least the following beneficial effects: the scheme of the present invention innovatively proposes to scientifically mix Patchouli alcohol with one or more of the natural active ingredients such as magnolol and borneol acetate to form an efficient antibacterial and anti-caries composition. The composition can be widely used in various oral care products, including but not limited to toothpaste, tooth powder, liquid toothpaste, mouthwash, tooth paste, chewing gum, oral spray and tooth gel, etc., aiming to provide users with all-round and multi-level oral health protection. The antibacterial and anti-caries composition proposed in the scheme of the present invention not only provides a new combination of active ingredients for oral care products, but also brings more comprehensive and efficient oral health protection to users through scientifically verified synergistic effects.

[0009] According to some embodiments of the invention, the composition consists of patchouli alcohol, magnolol, citral, ethyl p-methoxycinnamate, bornyl acetate and β-caryophyllene.

[0010] During use, these active ingredients show significant synergistic effects. Patchouli alcohol, with its unique antibacterial properties, works together with magnolol (a biphenol compound with a wide antibacterial spectrum), citral (an aldehyde compound with strong antibacterial and antioxidant effects), ethyl p-methoxycinnamate (an ester compound with antibacterial and anti-inflammatory activity), bornyl acetate (an ester compound with fresh breath and antibacterial effects) and β-caryophyllene (an olefin compound with antibacterial and anti-inflammatory potential) to form a powerful antibacterial barrier, effectively inhibiting the growth of various harmful bacteria in the oral cavity, especially Streptococcus mutans, the main pathogenic bacteria that causes dental caries. The antibacterial and anti-caries composition of the present invention not only significantly inhibits the growth of Streptococcus mutans and effectively prevents the occurrence of dental caries, but also has the potential to prevent and treat dental caries and periodontal disease due to its multiple protective effects. These active ingredients reduce the number of harmful bacteria by regulating the balance of oral microecology, and may promote the growth of beneficial bacteria, thereby maintaining oral health. In addition, they may further play a role in treating periodontal disease by regulating oral immune responses, reducing inflammatory responses, and other pathways.

[0011] According to some embodiments of the present invention, the patchouli alcohol is derived from chemical synthesis or natural product extraction.

[0012] According to some embodiments of the present invention, magnolol, citral, ethyl p-methoxycinnamate, bornyl acetate, and β-caryophyllene are derived from chemical synthesis or natural product extraction.

[0013] According to some embodiments of the present invention, the mass percentage of patchouli alcohol in the composition is 6% to 99.9%.

[0014] According to some embodiments of the present invention, the mass ratio of magnolol, citral, ethyl p-methoxycinnamate, bornyl acetate and β-caryophyllene is 1:8-27:8-27:129-427:32-107.

[0015] According to some embodiments of the present invention, the composition consists of the following parts by weight of patchouli alcohol, magnolol, citral, ethyl p-methoxycinnamate, borneol acetate and β-caryophyllene: 0.00025-0.016 parts of patchouli alcohol, 0.00031-0.006 parts of magnolol, 0.0025-0.16 parts of citral, 0.0025-0.16 parts of ethyl p-methoxycinnamate, 0.04-2.56 parts of borneol acetate, and 0.01-0.64 parts of β-caryophyllene.

[0016] According to the application of the second aspect of the embodiment of the present invention, there is provided an oral care product comprising a base material and the above composition.

[0017] According to the application of the embodiment of the present invention, at least the following beneficial effects are achieved: the composition of the scheme of the present invention is not only suitable for toothpaste, but also can be widely used in a variety of oral care products such as tooth powder, liquid toothpaste, mouthwash, tooth paste, chewing gum, oral spray and tooth gel. For the preparation of these products, it is only necessary to add a composition containing patchouli alcohol and one or more compounds of magnolol, borneol acetate, etc. to the corresponding formula according to the conventional method of the prior art. The oral care product using the composition of the scheme of the present invention has a good anti-caries effect and has broad prospects for industrial application.

[0018] According to some embodiments of the present invention, the oral care product comprises at least one of toothpaste, tooth powder, liquid toothpaste, mouthwash, tooth paste, chewing gum, oral spray or tooth gel.

[0019] According to some embodiments of the present invention, the oral care product is toothpaste, and the base material comprises a moisturizer, an abrasive, a thickener, a foaming agent, a sweetener, a flavor and a preservative.

[0020] According to some embodiments of the present invention, the humectant includes but is not limited to at least one of glycerol, propylene glycol, diethylene glycol, sorbitol or polyethylene glycol.

[0021] According to some embodiments of the present invention, the abrasive includes but is not limited to at least one of calcium carbonate, hydrated silica, silicon dioxide, calcium pyrophosphate or hydroxyapatite.

[0022] According to some embodiments of the present invention, the thickener includes but is not limited to at least one of sodium carboxymethyl cellulose, xanthan gum, carrageenan, nonionic guar gum, sodium alginate, hydroxyethyl cellulose or carbomer.

[0023] According to some embodiments of the present invention, the foaming agent includes but is not limited to at least one of sodium lauryl sulfate, sodium lauroyl sarcosinate, sodium lauryl sulfoacetate or cocopropyl betaine.

[0024] According to some embodiments of the present invention, the sweetener includes but is not limited to at least one of saccharin sodium, monk fruit extract, xylitol or glycerol.

[0025] According to some embodiments of the present invention, the flavor includes but is not limited to at least one of menthol, peppermint oil, spearmint or cardamom.

[0026] According to some embodiments of the invention, the preservative includes but is not limited to at least one of ethylparaben, propylparaben or sodium benzoate.

[0027] According to some embodiments of the present invention, the toothpaste comprises the following raw materials in parts by weight:

[0028] 0.00056-3.542 parts of anti-caries oral care composition

[0029] 70-90 parts of base material.

[0030] According to some embodiments of the present invention, the toothpaste comprises the following raw materials in parts by weight:

[0031] 0.00056-3.542 parts of anti-caries oral care composition

[0032] Moisturizer 10-70 parts

[0033] Friction agent 20-60 parts

[0034] Thickener 0.1-10 parts

[0035] Foaming agent 0.1-10 parts

[0036] Sweetener 0.1-2 parts

[0037] 0.1-5 parts of flavor

[0038] Preservative 0.1-1 part.

[0039] According to some embodiments of the present invention, the toothpaste comprises the following raw materials in parts by weight:

[0040] Baiqiuli alcohol 0.00025-0.016 parts

[0041] Magnolol 0.000310-0.006 parts

[0042] Citral 0.0025-0.16 parts

[0043] Ethyl p-methoxycinnamate 0.0025-0.16 parts

[0044] Bornyl acetate 0.04-2.56 parts

[0045] β-Caryophyllene 0.01-0.64 parts

[0046] Moisturizer 10-70 parts

[0047] Friction agent 20-60 parts

[0048] Thickener 0.1-10 parts

[0049] Foaming agent 0.1-10 parts

[0050] Sweetener 0.1-2 parts

[0051] 0.1-5 parts of flavor

[0052] Preservative 0.1-1 part.

[0053] According to some embodiments of the present invention, the raw materials of the toothpaste further include water, and the total mass of the raw materials is 100 parts, with water being the balance.

[0054] According to the application of the second aspect of the present invention, there is also provided a method for preparing an oral care toothpaste, comprising the following steps:

[0055] S1, dispersing the thickener in the humectant to form a mixed solution A after swelling;

[0056] S2, adding part of water to the above composition and mixing to form a mixed solution B;

[0057] S3, adding a sweetener, a preservative and the remaining water to the mixed solution A to obtain a mixed solution C;

[0058] S4, mixing the mixed solution C with the mixed solution B to form a mixed material D, and then aging it;

[0059] S5, adding a friction agent to the mixture D and mixing to obtain a mixture E;

[0060] S6, adding a foaming agent to the mixed material E and mixing the mixture to obtain a mixed material F;

[0061] S7. Add essence to the mixture F to obtain the oral care toothpaste.

[0062] The preparation method according to the embodiment of the present invention has at least the following beneficial effects: the toothpaste preparation process of the scheme of the present invention is simple and has good production and application prospects. In the preparation process, first ensure that the thickener and the humectant are fully dispersed and swollen, and build a stable framework structure of the toothpaste on this basis. Subsequently, select one or more compounds of patchouli alcohol and magnolol, citral, ethyl p-methoxycinnamate, bornyl acetate and β-caryophyllene, mix them thoroughly and dissolve them in water. This process aims to enhance the effectiveness of these ingredients in anti-caries and antibacterial effects. After completing the above steps, the mixture is mixed with other necessary ingredients to ensure the final stability of the toothpaste and the full play of the efficacy of each active ingredient.

[0063] Additional aspects and advantages of the present invention will be given in part in the following description and in part will be obvious from the following description, or will be learned through practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0064] The present invention will be further described below with reference to the accompanying drawings and embodiments, wherein:

[0065] Figure 1 This is a schematic diagram of the effect of the raw material patchouli alcohol used in the examples of the present invention on the growth curve of Streptococcus mutans. DETAILED DESCRIPTION

[0066] The following will be combined with the embodiments to clearly and completely describe the concept of the present invention and the technical effects produced, so as to fully understand the purpose, characteristics and effects of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of them. Based on the embodiments of the present invention, other embodiments obtained by technicians in this field without creative work are all within the scope of protection of the present invention. The test methods used in the embodiments are conventional methods unless otherwise specified; the materials, reagents, etc. used, unless otherwise specified, can be reagents and materials obtained from commercial channels. Unless otherwise specified, the same parameter in each embodiment has the same value. The embodiments described below are exemplary and are only used to explain the present invention, and cannot be understood as limitations on the present invention.

[0067] In the description of the present invention, the description with reference to the term "some embodiments" or the like means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.

[0068] In the description of the present invention, if there is a description of first, second, etc., it is only for the purpose of distinguishing technical features, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features or implicitly indicating the order of the indicated technical features.

[0069] Patchouli alcohol and magnolol, citral, ethyl p-methoxycinnamate, borneol acetate and β-caryophyllene in the embodiments of the present invention can all be purchased through commercial means. Patchouli alcohol, magnolol, citral and borneol acetate used in the embodiments are purchased from Shanghai Yuanye Biotechnology Co., Ltd.; ethyl p-methoxycinnamate and β-caryophyllene are extracted by essential oil extraction methods such as steam distillation and supercritical carbon dioxide fluid extraction to obtain essential oils, and then crystallized to obtain monomer compounds.

[0070] Ethyl p-methoxycinnamate is obtained by crystallization of Kaempferia galanga essential oil extracted by supercritical carbon dioxide. The extraction conditions of Kaempferia galanga essential oil are as follows: the pressure of the extraction kettle is 22MPa, the temperature of the extraction kettle is 55℃, and the extraction time is 2h. Other extraction conditions are as follows: the pressure of the separation kettle is 6MPa, the temperature is 40℃ and 30℃ respectively, and the CO2 flow rate is 30kg / h. After the essential oil is left to stand, a crystal precipitate is produced. The crystal is compared with the standard product by liquid chromatography / gas chromatography. The crystal is ethyl p-methoxycinnamate with a purity of ≥95%.

[0071] β-Caryophyllene is derived from the crystallization of the essential oil of the spice Osmanthus fragrans extracted by steam distillation. The extraction method of Osmanthus fragrans is the commonly used steam distillation method in the laboratory, with a solid-liquid ratio of 1:5 to 1:10. The extracted essential oil is allowed to stand to produce crystals. The crystals are compared with the standard using a liquid chromatograph / gas chromatograph, and the crystals are β-caryophyllene with a purity ≥95%.

[0072] Patchouli alcohol, magnolol and citral are ≥99.8%, the purity of borneol acetate is ≥99.5%, and purified water is used.

[0073] The "room temperature" referred to in the present invention refers to 25±5°C, and is specifically 25°C in the embodiments.

[0074] Example 1

[0075] This example provides an anti-caries oral care composition, which is composed of the following components in weight percentage: 0.01 parts of Patchouli alcohol and 0.003 parts of Magnolia officinalis.

[0076] This example also provides a toothpaste, which is made of the above composition, abrasive, thickener, moisturizing agent, sweetener, foaming agent, preservative, essence and water. The weight percentages of each raw material are: 0.013 parts of the composition, 10-70 parts of the moisturizing agent, 20-60 parts of the abrasive, 0.1-10 parts of the thickener, 0.1-10 parts of the foaming agent, 0.1-2 parts of the sweetener, 0.1-5 parts of the essence, 0.1-1 part of the preservative, and the balance of water.

[0077] The content of the moisturizer ranges from 10 to 70 parts, including but not limited to one or more of glycerin, propylene glycol, diethylene glycol, sorbitol, polyethylene glycol, and the like.

[0078] The content of the abrasive agent ranges from 20 to 60 parts, including but not limited to one or more of calcium carbonate, hydrated silica, silicon dioxide, calcium pyrophosphate, hydroxyapatite and the like.

[0079] The content of the thickener ranges from 0.1 to 10 parts, including but not limited to one or more of sodium carboxymethyl cellulose, xanthan gum, carrageenan, nonionic guar gum, sodium alginate, hydroxyethyl cellulose, carbomer, and the like.

[0080] The content of the foaming agent ranges from 0.1 to 10 parts, including but not limited to one or more of sodium lauryl sulfate, sodium lauroyl sarcosinate, sodium lauryl sulfoacetate, cocopropyl betaine, and the like.

[0081] The content of the sweetener ranges from 0.1 to 2 parts, including but not limited to one or more of saccharin sodium, monk fruit extract, xylitol, glycerin, and the like.

[0082] The content of the flavor ranges from 0.1 to 5 parts, including but not limited to one or more of menthol, peppermint oil, spearmint, cardamom, etc.

[0083] The content of preservatives ranges from 0.1 to 1 parts, including but not limited to one or more of ethylparaben, propylparaben, sodium benzoate, etc.

[0084] The preparation method of toothpaste is as follows:

[0085] S1: Disperse the thickener evenly in the moisturizer and form a mixed solution A after fully swelling;

[0086] S2: After fully mixing the components in the composition, dissolving them with appropriate amount of water into a mixed solution B with a mass fraction of 5%-15%;

[0087] S3: adding a sweetener, a preservative and an appropriate amount of water to the mixed solution A, and stirring evenly to obtain a mixed solution C;

[0088] S4: After the mixed solution C and the mixed solution B are fully stirred and mixed to form a mixed material D, the mixed material D is fully aged;

[0089] S5: adding a friction agent to the mixture D and mixing thoroughly to obtain a mixture E;

[0090] S6: adding a foaming agent to the mixture E and mixing thoroughly to obtain a mixture F;

[0091] S7: adding essence to the mixed material F, homogenizing and degassing to obtain the product, and then filling it into toothpaste in a conventional manner.

[0092] Example 2

[0093] This example provides an anti-caries oral care composition and toothpaste, which differs from Example 1 in that the total weight of the composition is 1.21 parts, and is specifically composed of the following components in parts by weight: 0.01 parts of patchouli alcohol and 1.2 parts of borneol acetate.

[0094] Example 3

[0095] This example provides an anti-caries oral care composition and toothpaste, which differs from Example 1 in that the total weight of the composition is 0.715 parts, and is specifically composed of the following components in parts by weight: 0.005 parts of patula alcohol, 0.01 parts of magnolol, 0.5 parts of borneol acetate, and 0.2 parts of β-caryophyllene.

[0096] Example 4

[0097] This example provides an anti-caries oral care composition and toothpaste, which differs from Example 1 in that the total weight of the composition is 0.815 parts, and is specifically composed of the following components in parts by weight: 0.005 parts of patula alcohol, 0.01 parts of magnolol, 0.05 parts of citral, 0.05 parts of ethyl p-methoxycinnamate, 0.5 parts of borneol acetate, and 0.2 parts of β-caryophyllene.

[0098] Comparative Example 1

[0099] This example provides a toothpaste, which differs from Example 1 in that the composition is replaced with 0.00025 parts of patchouli alcohol.

[0100] Comparative Example 2

[0101] This example provides a toothpaste, which differs from Example 1 in that the composition is replaced with 0.01 parts of patchouli alcohol.

[0102] Comparative Example 3

[0103] This example provides a toothpaste, which differs from Example 1 in that the composition is replaced with 0.025 parts of patchouli alcohol.

[0104] Comparative Example 4

[0105] This example provides an anti-caries oral care composition and toothpaste, which differs from Example 1 in that the total weight of the composition is 0.11 parts, and is specifically composed of the following components in parts by weight: 0.01 parts of patchouli alcohol and 0.1 parts of citral.

[0106] Comparative Example 5

[0107] This example provides an anti-caries oral care composition and toothpaste, which differs from Example 1 in that the total weight of the composition is 0.11 parts, and is specifically composed of the following components in parts by weight: 0.01 parts of patchouli alcohol and 0.1 parts of ethyl p-methoxycinnamate.

[0108] Comparative Example 6

[0109] This example provides an anti-caries oral care composition and toothpaste, which differs from Example 1 in that the total weight of the composition is 0.31 parts, and is specifically composed of the following components in parts by weight: 0.01 parts of patchouli alcohol and 0.3 parts of β-caryophyllene.

[0110] The toothpaste formulas in the embodiments and comparative examples are specifically shown in Table 1 below:

[0111] Table 1 Antibacterial and anti-caries toothpaste formula (unit: mass percentage)

[0112]

[0113]

[0114] The total mass percentage of toothpaste is 100%. When the sum of the mass percentages of other toothpaste raw materials is less than 100%, the remainder is supplemented with water.

[0115] Test Case

[0116] This example tests the anti-caries effect of the toothpaste. The specific operation is to take the toothpaste prepared in the above embodiment and comparative example and test its antibacterial effect on Streptococcus mutans.

[0117] 1) Preparation of Streptococcus mutans suspension

[0118] The activated standard strain of Streptococcus mutans (ATCC 25175, commercially available) was picked and inoculated on the RCA plate and evenly spread, then inverted and placed in an anaerobic bag. After culturing in a 37°C incubator for 24 hours, the bacterial moss was scraped from the plate with a disposable sterile inoculation loop, suspended in sterile PBS to prepare a bacterial solution, and streaked on the RCA plate for culturing. After anaerobic culture for 24 hours, a single colony was picked and anaerobically cultured in a BHI liquid culture medium at 37°C and 180 rpm in a shaking incubator; the bacteria in the logarithmic growth period were taken and the absorbance (OD) was adjusted to 1.0 at a wavelength of 600 nm using an ultraviolet spectrophotometer, and used as the standard bacterial solution for later use.

[0119] 2) Test on the growth curve of Streptococcus mutans by using Patchouli alcohol

[0120] The experimental groups diluted Patchouli alcohol to MIC and below (1 / 2MIC, 1 / 4MIC, 1 / 8MIC) three concentrations, took 1mL and added to the test tubes, and then added 1mL of working bacterial solution diluted 100 times with the standard bacterial solution. The bacterial solution control group (Control) added DMSO solution and bacterial solution with the same concentration as the MIC group. Each group was set up with 6 parallel groups; one tube was taken out at 0, 4, 8, 12, 24, and 48 hours, and the OD was measured 600 Draw a growth curve.

[0121] Growth curve Figure 1 As shown in the figure, compared with the control group, Patchouli alcohol can significantly inhibit the time for Streptococcus mutans to reach the plateau phase. The control group entered the logarithmic growth phase at 4h and reached the plateau phase at 12h; the MIC group entered the logarithmic growth phase at 8h and reached the plateau phase at 24h; the 1 / 2MIC group and the 1 / 4MIC group entered the logarithmic growth phase at 4h and reached the plateau phase at 24h.

[0122] 3) Combined drug sensitivity test of Patchouli alcohol and other active ingredients

[0123] Using Streptococcus mutans as the indicator bacterium, the minimum inhibitory concentrations (MICs) of patchouli alcohol, magnolol, citral, ethyl p-methoxycinnamate, bornyl acetate, and β-caryophyllene were determined. The MICs of patchouli alcohol and each compound were diluted by 2, 1, 1 / 2, 1 / 4, 1 / 8, 1 / 16, and 1 / 32 times using BHI medium and a checkerboard method was used to conduct a 7×7 combination test. The bacterial suspension concentration was set the same as in the part of the test for the growth curve determination of patchouli alcohol against Streptococcus mutans. The optimal combined effect concentration was selected and the fractional inhibitory concentration index (FICI) was calculated.

[0124] The calculation formula for FICI is as follows:

[0125]

[0126] Judgment criteria: FICI ≤ 0.5, synergistic effect; 0.5 < FICI ≤ 1, additive effect; 1 < FICI ≤ 2, no effect; FICI > 2, antagonistic effect.

[0127] The test results showed that the MIC value of patchouli alcohol was 40 μg / ml, the MIC value of magnolol was 12.5 μg / ml, the MIC value of citral was 400 μg / ml, the MIC value of ethyl p-methoxycinnamate was 400 μg / ml, the MIC value of bornyl acetate was 6.4 mg / ml, and the MIC value of β-caryophyllene was 1.6 mg / ml.

[0128] The combined drug sensitivity test showed that:

[0129] For patchouli alcohol and magnolol, the optimal combined effect concentration was 1 / 16 MIC concentration of patchouli alcohol and 1 / 4 MIC concentration of magnolol, and the FICI value was 0.3125, indicating that the combined use of patchouli alcohol and magnolol had a synergistic effect on the antibacterial effect against Streptococcus mutans.

[0130] For patchouli alcohol and bornyl acetate, the optimal combined effect concentration was 1 / 16 MIC concentration of patchouli alcohol and 1 / 4 MIC concentration of bornyl acetate, and the FICI value was 0.3125, indicating that the combined use of patchouli alcohol and bornyl acetate had a synergistic effect on the antibacterial effect against Streptococcus mutans.

[0131] For patchouli alcohol and citral, the optimal combined effect concentration was MIC concentration of patchouli alcohol and MIC concentration of citral, and the FICI value was 2, indicating that the combined use of patchouli alcohol and citral had no effect on the antibacterial effect against Streptococcus mutans.

[0132] For patula alcohol and ethyl p-methoxycinnamate, the optimal combined effect concentration was 1 / 2MIC concentration of patula alcohol and MIC concentration of ethyl p-methoxycinnamate, and the FICI value was 1.5, indicating that the combined use of patula alcohol and ethyl p-methoxycinnamate had no effect on the inhibition of Streptococcus mutans.

[0133] For patchouli alcohol and β-caryophyllene, the optimal combination effect concentration was 1 / 2MIC concentration of patchouli alcohol and 1 / 4MIC concentration of β-caryophyllene, and the FICI value was 0.75, indicating that the combined use of patchouli alcohol and β-caryophyllene had an additive effect on the antibacterial effect of Streptococcus mutans.

[0134] 4) Evaluation test on the antibacterial effect of compound antibacterial and anti-caries toothpaste containing Patchouli alcohol

[0135] The antibacterial effect of the toothpaste in the examples and comparative examples was investigated by referring to "5.1.2 Carrier Immersion Quantitative Antibacterial Test" in the "Health Industry Standards of the People's Republic of China". Mutans Streptococcus was diluted with PBS to about 5×10 6 CFU / mL~5×10 7 CFU / mL is used to make a bacterial suspension for later use. Take 10μL of the bacterial suspension on a drug-sensitive paper, dry it at 36℃±1℃ or air it at room temperature for later use. Weigh 5g / piece of the toothpaste sample prepared in the embodiment or comparative example into a sterile plate, place it in a 20℃±1℃ water bath for 5min, take the above-mentioned drug-sensitive paper with sterile tweezers, and immerse the carrier completely in the sample, and time it for 5min. Then take out the drug-sensitive paper and add it to a 5.0mL PBS test tube, mix it, oscillate it, wash off the test bacteria, absorb 1.0mL of the sample solution, and determine the number of surviving bacteria according to the live bacteria culture counting method. Inoculate 2 plates with each tube of sample solution. If the number of colonies growing on the plate is large, PBS can be used for 10-fold serial dilution, and then live bacteria culture counting can be performed. Take 10.0g of blank toothpaste matrix that does not contain antibacterial and anti-caries active ingredients and soak it in 2 drug-sensitive paper sheets for parallel experiments as a positive control. The amount of bacteria recovered in the positive control is 1.0×10 4 CFU / piece~9.0×10 4 CFU / piece. Take PBS and culture medium from the same batch as negative control. All test samples and control samples were cultured at 36℃±1℃, and the results were observed for 24 hours. The test was repeated 3 times and the inhibition rate was calculated.

[0136] The antibacterial rate calculation method is as follows:

[0137]

[0138] Where:

[0139] X—inhibition rate, %;

[0140] A0—average colony count of control samples, in CFU / piece;

[0141] A1—Average colony count of the tested samples, in CFU / piece.

[0142] The test results are shown in Table 2.

[0143] Table 2 Test results of antibacterial rate of toothpaste against Streptococcus mutans in Examples and Comparative Examples

[0144]

[0145]

[0146] If the inhibition rate is ≥50% to 90%, it is judged to have an antibacterial effect; if the inhibition rate is ≥90%, it is judged to have a strong antibacterial effect.

[0147] The test results show that the embodiments of the present invention all have antibacterial effects, especially when multiple components are compounded together, the effect can be significantly improved to more than 99.6%.

[0148] 5) Toothpaste quality evaluation

[0149] The quality of the antibacterial and anti-caries toothpaste containing Patchouli alcohol prepared by the method of the embodiment was tested. With reference to the sensory and physical and chemical indicators in GB / T8372-2017 Toothpaste, the quality evaluation was carried out using the paste form, stability and foam volume as a comprehensive evaluation method.

[0150] Evaluation of forming condition and paste morphology: Take a toothpaste sample, squeeze 2cm from a 8mm diameter mouth onto a toothbrush. The toothpaste prepared in this embodiment is easy to squeeze out, has obvious wire drawing, is easy to cut, and has no obvious collapsed area; the paste is clean and delicate, with uniform color, bright and free of impurities.

[0151] Stability evaluation: Take 2 toothpaste samples, store one sample at room temperature; put the other sample into a refrigerator at (-8±1)℃ for 8 hours, then take it out, and then put it into a constant temperature incubator at (45±1)℃ for 8 hours, then take it out, restore it to room temperature, open the cover, the paste should not overflow from the tube, turn the toothpaste tube upside down, and no liquid should drip from the tube within 10 seconds; compare the paste with the room temperature sample after squeezing it out. The toothpaste prepared in this embodiment does not overflow from the tube, does not separate liquid, and the fragrance body has normal color.

[0152] Foam volume evaluation: Pre-weigh 45°C, 20mL water, weigh 1g of the toothpaste to be tested in a beaker, add a small amount of water to dissolve the paste, pour the dissolved paste into a stoppered measuring cylinder, wash the beaker with the remaining water, pour it into the measuring cylinder, cover and press the stopper tightly, shake the solution in the measuring cylinder with the maximum force, stop after the paste is completely dissolved, place the measuring cylinder on the operating table and let it stand for 5 minutes, record the foaming amount based on the most concentrated position of the foam distribution in the measuring cylinder, repeat 3 times, and take the average value. The toothpaste foam volume prepared in this embodiment is ≥90mL, which meets the corresponding national standards. The toothpaste foam volume prepared in each embodiment of the present invention is ≥90mL, which meets the corresponding national standards.

[0153] The mechanism of action of each component in the anti-caries oral care composition of the present invention is speculated as follows:

[0154] The patchouli alcohol in the composition of the present invention exhibits excellent water solubility and compatibility with a variety of organic solvents (including alcohols, ethers and esters), which greatly broadens its convenience of use and scope of application. Patchouli alcohol is derived from the traditional medicinal material Patchouli, which is both a medicine and food. As its main active ingredient, it is not only low-cost and widely available, but also has excellent biosafety. In terms of pharmacological effects, patchouli alcohol exhibits a broad spectrum of antibacterial activity, including inhibition of bacteria and fungi, and the ability to resist other pathogenic microorganisms, especially in the treatment of infections caused by Helicobacter pylori and Candida albicans, patchouli alcohol shows good therapeutic effects. In addition, for the main pathogenic bacteria of dental caries, Streptococcus mutans, the present invention unexpectedly found that patchouli alcohol also has a significant inhibitory effect on it. Therefore, the application of patchouli alcohol in oral care products can effectively inhibit bacterial growth, prevent dental caries, and achieve ideal antibacterial and anti-caries effects.

[0155] Magnolol, as the key active ingredient of the traditional Chinese medicine Magnolia officinalis, is classified as a biphenol compound and exhibits a wide range of inhibitory activity against a variety of bacteria. In recent years, the research focus on magnolia officinalis in the field of oral health has mainly focused on its inhibitory effect on Streptococcus mutans, the main pathogen causing caries, thereby effectively delaying the progression of caries. Its antibacterial and anti-inflammatory mechanisms may involve regulating signal transduction pathways such as tumor necrosis factor TNF-α, phosphatidylinositol 3-kinase / protein kinase B (PI3K / Akt) and mitogen-activated protein kinase (MAPK), thereby exerting an anti-inflammatory effect. In addition, magnolia officinalis can also regulate the expression balance of osteoprotegerin (OPG) and receptor activator of nuclear factor κB ligand (RANKL), which helps to reduce alveolar bone resorption and promote bone regeneration, which has positive significance for alleviating clinical symptoms related to periodontitis. Given the excellent anti-Streptococcus mutans performance of magnolia officinalis, it has been widely incorporated into the formula of a variety of oral care products.

[0156] Bornyl acetate, as the main component of Amomum villosum volatile oil, is not only widely used in the field of spices, but also used in cosmetics, soaps, indoor disinfectants, air fresheners, indoor spray fragrances, bath fragrances and talcum powders to add its aromatic properties. It also shows potential positive effects in oral health care, especially in the prevention of dental caries. Bornyl acetate has certain antibacterial properties and can inhibit some harmful microorganisms in the mouth. Bacteria in the mouth, such as Streptococcus mutans, are one of the main causes of dental caries. They produce acidic substances through metabolism, corrode the hard tissues of teeth, and cause the occurrence of dental caries. Bornyl acetate can reduce the erosion of teeth by inhibiting the activity of these harmful bacteria, thereby helping to prevent the occurrence of dental caries. In addition, the fresh aroma of bornyl acetate can also improve the oral environment and enhance the comfort of users. Therefore, the reasonable addition of bornyl acetate to oral care products can not only improve the product experience, but also enhance the anti-caries effect of the product to a certain extent.

[0157] Ethyl p-methoxycinnamate is a main component of Kaempferia galanga (a plant). Existing research results show that this compound exhibits good antibacterial effects on Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Candida albicans and Aspergillus niger. Further research in this technical solution found that ethyl p-methoxycinnamate also has a strong inhibitory effect on Streptococcus mutans. Therefore, ethyl p-methoxycinnamate has certain application potential in the development of oral care products.

[0158] Citral, whose chemical name is 3,7-dimethyl-2,6-octadienal, is a colorless to slightly yellow liquid with a strong lemon aroma. Citral in nature is mainly composed of two monoterpenoid isomers and is widely distributed in plants such as lemongrass, verbena, and Litsea cubeba. This compound exhibits a variety of biological activities, including but not limited to antiseptic and antibacterial, insecticidal, anti-inflammatory, potential anticancer and antioxidant effects. In the food industry, citral has attracted much attention due to its significant antibacterial and antifungal activities.

[0159] The β-caryophyllene involved in the scheme of the present invention is the main component of the essential oil extracted from the seasoning Murraya paniculata by steam distillation, and then a pure substance obtained by a crystallization purification process. According to in-depth research on this technical solution, β-caryophyllene has shown a significant inhibitory effect on Streptococcus mutans, a common cariogenic bacteria in the oral cavity. The antibacterial mechanism of β-caryophyllene can inhibit its growth and reproduction by interfering with the metabolic process of Streptococcus mutans or destroying the integrity of its cell membrane. By reducing the number of Streptococcus mutans in the oral cavity, β-caryophyllene helps to reduce the production of acidic substances, reduce the corrosive effect on teeth, and thus play a role in preventing dental caries. Therefore, the application of β-caryophyllene in oral care products, such as toothpaste, mouthwash, etc., can not only utilize its natural antibacterial properties to effectively inhibit the growth of cariogenic bacteria such as Streptococcus mutans, but also provide consumers with a safer and natural anti-caries solution.

[0160] In summary, the embodiments of the present invention provide an anti-caries oral care composition containing Patchouli alcohol, and the oral care products prepared therefrom have multiple advantages: the formula design is scientific, the raw materials are widely available, the use is safe and reliable, and a fresh smell is emitted. In addition, the composition exhibits excellent biosafety, can effectively inhibit the growth of dental plaque, maintain oral hygiene and hygiene for a long time, and exerts a significant antibacterial and antibacterial effect, thereby refreshing breath and maintaining oral health.

[0161] The embodiments of the present invention are described in detail above, but the present invention is not limited to the above embodiments. Various changes can be made within the knowledge scope of ordinary technicians in the relevant technical field without departing from the purpose of the present invention.

Claims

1. An anti-caries oral care composition, characterized in that: The invention comprises component A, component B and component C, wherein component A is patchouli alcohol, component B is at least one of magnolol and bornyl acetate, and component C comprises at least one of citral, ethyl p-methoxycinnamate or β-caryophyllene; wherein the contents of component A and component B are greater than zero, and the content of component C is greater than or equal to zero.

2. The anti-caries oral care composition according to claim 1, characterized in that: The composition consists of patula alcohol, magnolol, citral, ethyl p-methoxycinnamate, bornyl acetate and beta-caryophyllene.

3. The anti-caries oral care composition according to claim 1 or 2, characterized in that: The mass percentage of patchouli alcohol in the composition is 6% to 99.9%.

4. The anti-caries oral care composition according to claim 2, characterized in that: The mass ratio of magnolol, citral, ethyl p-methoxycinnamate, bornyl acetate and beta-caryophyllene is 1:8-27:8-27:129-427:32-107.

5. The anti-caries oral care composition according to claim 2, characterized in that: The composition consists of the following weight proportions of patchouli alcohol, magnolol, citral, ethyl p-methoxycinnamate, borneol acetate and β-caryophyllene: 0.00025-0.016 part of patchouli alcohol, 0.000310-0.006 part of magnolol, 0.0025-0.16 part of citral, 0.0025-0.16 part of ethyl p-methoxycinnamate, 0.04-2.56 parts of borneol acetate and 0.01-0.64 part of β-caryophyllene.

6. An oral care product, characterized in that: The method comprises a base material and the composition according to any one of claims 1 to 5.

7. The oral care product according to claim 6, characterized in that: The oral care product includes at least one of toothpaste, tooth powder, liquid toothpaste, mouthwash, tooth paste, chewing gum, oral spray or tooth gel.

8. The oral care product according to claim 6, characterized in that: The oral care product is toothpaste, and the base material comprises a preservative, an abrasive, a thickener, a foaming agent, a sweetener, a flavor and a preservative.

9. The oral care product according to claim 8, characterized in that: The toothpaste comprises the following raw materials in parts by weight: 0.00056-3.542 parts of anti-caries oral care composition Moisturizer 10-70 parts Friction agent 20-60 parts Thickener 0.1-10 parts Foaming agent 0.1-10 parts Sweetener 0.1-2 parts 0.1-5 parts of flavor Preservative 0.1-1 part.

10. A method for preparing an oral care toothpaste, characterized in that: The steps include: S1, dispersing the thickener in the humectant to form a mixed solution A after swelling; S2, adding part of water to the composition according to any one of claims 1 to 5 and mixing to form a mixed solution B; S3, adding a sweetener, a preservative and the remaining water to the mixed solution A to obtain a mixed solution C; S4, mixing the mixed solution C with the mixed solution B to form a mixed material D, and then aging it; S5, adding a friction agent to the mixture D and mixing to obtain a mixture E; S6, adding a foaming agent to the mixed material E and mixing the mixture to obtain a mixed material F; S7. Add essence to the mixture F to obtain the oral care toothpaste.

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