Composition containing rhizoma drynariae extract and capable of enhancing anti-acid repairing effect, oral care product and preparation method of oral care product

Abstract

The invention relates to the technical field of oral care products, in particular to an anti-acid repairing oral care composition, application thereof and an oral care product containing the composition. The anti-acid repairing oral care composition comprises strontium ions and a rhizoma drynariae extract, the preparation method comprises the following steps: mixing soluble strontium salt with water to obtain a strontium ion system; mixing the rhizoma drynariae extract with a humectant to obtain a rhizoma drynariae system; and mixing the strontium ion system and the rhizoma drynariae system, and performing ultrasonic treatment. The anti-acid repairing oral care composition can be applied to preparation of oral care products including toothpaste. According to the technical scheme, on the premise that potential allergens are prevented from being introduced and the stability of the product in the storage and use process is ensured, the bioavailability and the acting effect of strontium ions are effectively improved, and then the technical problem that the bioavailability and the acting effect of the strontium ions of the strontium-containing anti-acid repairing oral care product are limited is solved; and the method has ideal application and popularization prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of oral care products, and in particular to a composition containing a rhizoma drynariae extract and having enhanced acid resistance and repairing effects, as well as an oral care product and a preparation method thereof. Background Art

[0002] Dentin hypersensitivity is a common symptom of tooth sensitivity, typically caused by a brief, intense pain caused by temperature changes, mechanical stimulation, or osmotic pressure fluctuations after the dentin surface is exposed. Its occurrence is often associated with the opening of dentinal tubules due to gum recession, enamel wear, or tooth neck defects. These tubules extend from the dental pulp to the cementum and are normally covered and protected. When exposed due to acid erosion, improper toothbrushing, or other reasons, external stimuli can activate the pulp nerves through the flow of fluid within the tubules, thereby triggering a pain response.

[0003] Strontium chloride, as a classic ingredient for combating dentin hypersensitivity, has been widely used in oral care products. It has a significant therapeutic effect on dentin hypersensitivity caused by wedge-shaped defects and root exposure due to gingival recession, and can effectively block and seal the openings of dentinal tubules. Despite this, strontium chloride still has certain limitations in practical applications, especially in terms of less than ideal bioavailability, and the efficiency of a single form of strontium salt in promoting remineralization still has room for improvement. Especially in the case of low strontium content, strontium salts have limited ability to promote dentin mineralization and enhance tooth resistance to acid erosion.

[0004] The applicant has previously attempted to increase the bioavailability of strontium by combining strontium ions with casein phosphopeptides. See prior patent CN115778838B (An oral care composition, its use, and oral care products containing the composition) for details. In this technical solution, the oral care composition includes strontium ions and casein phosphopeptides. Combining casein phosphopeptides with soluble strontium salts can increase the bioavailability of the strontium salts, increasing the adsorption and delivery of strontium ions to the tooth surface. This technical solution overcomes the technical problem of unsatisfactory effects of strontium ions in oral care products due to the difficulty in further increasing their concentration. Furthermore, casein phosphopeptides synergize with strontium to combat tooth erosion and enhance tooth remineralization. However, the above technical solution still has the following drawbacks: Casein phosphopeptides are a type of bioactive peptide produced by enzymatic hydrolysis of proteins. They may retain some allergenic epitopes, posing the risk of triggering allergic reactions. This can induce varying degrees of immune responses, especially in individuals sensitive to these proteins. Therefore, casein phosphopeptides are considered a potential allergen. Furthermore, the phosphate groups on casein phosphopeptides are susceptible to environmental factors (such as temperature, pH, light, and prolonged storage) during storage and application, potentially leading to denaturation or inactivation, resulting in decreased functional stability. Strontium-containing oral care products in the prior art still present several technical challenges. First, the bioavailability of strontium ions in the oral environment is limited. Especially at low strontium content, the effectiveness of strontium salts in promoting dentin mineralization and improving tooth resistance to acid erosion is less than ideal. Second, to enhance the efficacy of strontium ions, the prior art often increases the concentration of strontium salts, but this often results in decreased product stability and the introduction of potential allergens. In addition, although various auxiliary ingredients have been tried in the prior art to enhance the effect of strontium ions, these combinations often have problems such as insufficient synergistic effect and poor biocompatibility.

[0005] Therefore, there is an urgent need to develop an oral care composition that can significantly improve the bioavailability of strontium ions and enhance the acid-resistant repair effect of strontium ions under low strontium content conditions, while having good biocompatibility, so as to address the deficiencies in the existing technology. Summary of the Invention

[0006] The present application intends to provide an anti-acid repair effect enhanced composition containing Rhizoma Drynariae extract, so as to effectively improve the bioavailability and effect of strontium ions while avoiding the introduction of potential allergens and ensuring the stability of the product during storage and use. In particular, in the case of lower strontium content, the promotion of dentin mineralization and the improvement of tooth acid erosion resistance by strontium salt is limited, and there is a risk of introducing potential allergens in the prior art. Therefore, the present technical solution provides an anti-acid repair oral care composition, which can solve the technical problems of limited bioavailability and effect of strontium ions in strontium-containing anti-acid repair oral care products, and achieve the technical effect of significantly improving the thickness of the mineralization layer and the anti-acid erosion protection ability of the teeth.

[0007] To achieve the above-mentioned purpose, the present application adopts the following technical solutions: An anti-acid repair effect enhanced composition containing Rhizoma Drynariae extract, comprising strontium ions and Rhizoma Drynariae extract.

[0008] Further, the mass ratio of strontium ions to Rhizoma Drynariae extract is (0.10-1.75):(0.10-5.00); preferably, the mass ratio of strontium ions to Rhizoma Drynariae extract is (0.10-1.75):(0.10-2.00).

[0009] Further, the content of naringin in the Rhizoma Drynariae extract is ≥20%.

[0010] Further, the strontium ions are provided in the form of soluble strontium salt; the soluble strontium salt includes at least one of the hydrates and non-hydrates of strontium acetate, strontium chloride, strontium nitrate, strontium lactate, and strontium bromide.

[0011] The present technical solution also provides an oral care product containing an anti-acid repair oral care composition, the mass ratio of strontium ions in the oral care product is 0.10-1.75%, and the mass ratio of Rhizoma Drynariae extract in the oral care product is 0.10-2.00%.

[0012] Further, the oral care product further comprises the following raw materials: humectant 15.00-65.00 parts, abrasive 0.00-55.00 parts, thickening agent 0.20-9.00 parts, surfactant 1.00-22.00 parts, sweetener 0.20-3.00 parts, essence 0.20-5.50 parts, and pH adjuster 0.10-0.35 parts.

[0013] Further, the humectant includes at least one of glycerol, sorbitol, polyethylene glycol (PEG), and propylene glycol; The abrasive includes at least one of silicon dioxide, calcium bicarbonate, and calcium hydrogen phosphate dihydrate; The thickener comprises at least one of sodium carboxymethyl cellulose, hydroxyethyl cellulose, carbomer, carrageenan, guar gum and xanthan gum; The surfactant comprises at least one of sodium lauryl sulfate, cocoyl alanine triacetate ammonium, cocamidopropyl betaine, potassium cocoyl glycinate, sodium cocoyl glycinate, sodium lauroyl sarcosinate, alkyl glucoside, sodium laureth sulfate and triethanolamine cocoyl glutamate; The sweetener comprises at least one of saccharin sodium, aspartame, stevia, sucralose, acesulfame potassium, sucrose and xylitol; The flavor comprises one of lemon flavor, fruit flavor, spearmint flavor, wintergreen flavor, peppermint and mint essential oil; The pH adjuster includes at least one of tetrasodium pyrophosphate, disodium dihydrogen pyrophosphate, sodium hydroxide, sodium bicarbonate and sodium tripolyphosphate.

[0014] Furthermore, the acid-resistant oral care composition is prepared by the following method: A soluble strontium salt is mixed with water in a mass ratio of 1:1-1:2 to obtain a strontium ion system; a drynaria extract is mixed with a moisturizer in a mass ratio of 1:1-1:3 to obtain a drynaria system; the strontium ion system and the drynaria system are mixed and then ultrasonically treated to obtain an acid-resistant repairing oral care composition; the parameters of the ultrasonic treatment are: ultrasonic power 150-250W, ultrasonic time 20-50min.

[0015] The present invention also provides a method for preparing an oral care product, comprising the following steps in sequence: S1: Soluble strontium salt and water are mixed in a mass ratio of 1:1-1:2 to obtain a strontium ion system; Mixing the drynaria extract and polyethylene glycol at a mass ratio of 1:1-1:3 to obtain a drynaria system; The strontium ion system and the drynaria system are mixed, and then ultrasonically treated to obtain an acid-resistant and repairing oral care composition; S2: sorbitol and the remaining polyethylene glycol are mixed, and a thickener is added and mixed evenly, and then the acid-resistant oral care composition, sweetener, surfactant, pH regulator and the remaining water are added and stirred evenly.

[0016] S3: Add the friction agent, stir evenly and then evacuate; finally add the essence, stir evenly and degas.

[0017] Furthermore, the soluble strontium salt is strontium chloride hexahydrate; the mass ratio of strontium chloride hexahydrate to drynaria extract is (0.30-5.32): (0.10-5.00); preferably, the mass ratio of strontium chloride hexahydrate to drynaria extract is (0.30-5.32): (0.10-2.00); The parameters of the ultrasonic treatment are: ultrasonic power 150-250W, ultrasonic time 20-50min; preferably, the ultrasonic power is 180W; and the ultrasonic time is 30min.

[0018] In summary, the technical principles of this technical solution are as follows: This invention achieves anti-acid repair benefits through the synergistic effect of strontium chloride hexahydrate and Drynaria extract. The technical principle of this solution is as follows: strontium chloride hexahydrate provides strontium ions, which can block dentinal tubules and participate in the mineralization process to form a protective layer, reducing the impact of external stimuli on the dental pulp nerves. However, when used alone, its mineralization efficiency and acid erosion resistance are limited. Active ingredients such as naringin (≥20%) contained in Drynaria extract promote the deposition and nucleation of mineralization-related ions, enhance the adsorption and retention of strontium ions on the dentin surface, and modulate the local microenvironment to optimize mineralization conditions. At a specific ratio (strontium chloride hexahydrate:0.10-1.75:0.10-2 by mass), the two, through intermolecular interactions (such as the coordination of strontium ions with the active ingredients in the extract), significantly increase the speed and thickness of the mineralized layer formation, while also enhancing acid erosion resistance, achieving a synergistic effect. By controlling the dosage of Drynaria extract, the paste stability is improved (the dosage of Drynaria extract in toothpaste should ideally not exceed 2%). This technical solution represents the first use of Drynaria extract and strontium salts in the preparation of oral care products. Ensuring the stability of their combination in the toothpaste system was a major challenge faced by the inventors. By preparing a preform of the combination, the compatibility and compatibility of Drynaria extract and strontium salt with other toothpaste ingredients can be improved.

[0019] In addition, ultrasonic treatment (150-250W, 20-50min) promotes uniform dispersion and full interaction of strontium chloride hexahydrate and Drynaria extract, preventing aggregation and ensuring stable release of active ingredients. It also improves the paste's microstructure and enhances storage stability. Drynaria extract can be unstable in complex formulations such as oral care products (such as toothpaste), especially at high temperatures, causing browning and other instabilities. Ultrasonic treatment of the strontium salt and Drynaria extract enhances their complexation and improves paste stability.

[0020] The beneficial effects of this technical solution are: (1) Significant synergistic performance When strontium chloride hexahydrate and Drynaria extract are used together, the mineralized layer thickness is significantly higher than when either component is used alone, as well as the theoretical combined value. This significantly increases the mineralized layer thickness, and the synergistic effect significantly enhances tooth protection against acid erosion. Furthermore, a significant synergistic effect is observed when the mass ratio of strontium chloride hexahydrate to Drynaria extract is within the range of (0.10-1.75):(0.10-2), representing the optimal range for synergistic effects.

[0021] (2) Excellent stability and safety Paste Stability: Ultrasonic pretreatment and controlled dosage of Drynaria extract (≤2 parts) prevent discoloration, agglomeration, or water separation at high dosages, ensuring the product's physical stability during storage (especially under high-temperature conditions). This technical solution is the first to combine Drynaria extract and strontium salts in the preparation of oral care products. Ensuring the stability of their combination in a toothpaste system was a major challenge faced by the inventors. By preparing a preform of the composition, the compatibility and compatibility of Drynaria extract and strontium salts with other toothpaste ingredients can be improved.

[0022] Improved safety: Compared with the existing solutions containing casein phosphopeptides, the present invention uses Drynaria extract (plant-derived), avoiding the introduction of potential allergens and reducing the risk of immune response. At the same time, the active ingredients are more stable and are not significantly affected by environmental factors such as temperature and pH.

[0023] (3) Superiority of ingredients The synergistic effect of Drynaria extract is better than that of pine bark extract, which proves that Drynaria extract has more advantages in enhancing the anti-acid repair effect.

[0024] In summary, the present invention has significant advantages in improving the acid-resistant repair performance, stability and safety of oral care products through the synergistic effect, precise ratio and key process of strontium chloride hexahydrate and drynaria extract, and solves the problems of low bioavailability of strontium ions, limited effect and potential allergic risks in the existing technology. DETAILED DESCRIPTION

[0025] The present invention will be further described in detail below with reference to the examples, but the embodiments of the present invention are not limited thereto. Unless otherwise specified, the technical means used in the following examples and experimental examples are conventional means well known to those skilled in the art, and the materials, reagents, etc. used are all commercially available.

[0026] The overall situation of this technical solution is as follows: An anti-acid repair oral care composition comprises strontium ions and drynaria extract in a mass ratio of (0.10-1.75):(0.10-5.00); preferably, the anti-acid repair oral care composition comprises strontium ions and drynaria extract in a mass ratio of (0.10-1.75):(0.10-2).

[0027] The strontium ions are provided in the form of a soluble strontium salt, which includes at least one of a hydrate and a non-hydrate of strontium acetate, strontium chloride, strontium nitrate, strontium lactate, and strontium bromide.

[0028] Drynaria is the rhizome of Drynaria fortunei (Kunze) J. Sm. Drynaria fortunei The drynaria extract is usually prepared using drynaria decoction pieces as raw materials, that is, the drynaria extract is prepared using dry rhizomes of Drynaria fortunei as raw materials. The drynaria decoction piece standard can be found in Chinese Pharmacopoeia 2020 Drynaria Rhizoma, which records that naringin is the marker component of drynaria medicinal materials. The main effective component and the marker component of the drynaria extract are naringin, which can be prepared by the following prior art method: after the drynaria decoction pieces are crushed, ethanol solution is added, and the drynaria decoction pieces are extracted by multiple extraction (ethanol solution reflux can also be used for extraction), the extract is collected, and the extract is purified by ultrafiltration, reverse osmosis, or column chromatography, etc. to enrich the marker component naringin. After the purified extract is concentrated into a thick paste, it is dried and crushed to obtain the dry drynaria extract. The drynaria extract can also be purchased through commercial means. There are a large number of drynaria extracts prepared by commercial extraction methods using ethanol as the solvent in the prior art. The main effective component and technical index of the drynaria extract are naringin, and the content of naringin in the drynaria extract should be >20%. In the specific application of the present technical solution, the drynaria extract is purchased from Yunnan Inge Biotechnology Co., Ltd., and the specific content of naringin is 25%. The content of naringin in the extract can be determined by a conventional high-performance liquid chromatography method.

[0029] An oral care product containing an anti-acid repair oral care composition comprises the following raw materials in parts by weight: anti-acid repair oral care composition 0.20-6.75 parts, humectant 15.00-65.00 parts, rubbing agent 0.00-55.00 parts, thickening agent 0.20-9.00 parts, surfactant 1.00-22.00 parts, sweetener 0.20-3.00 parts, essence 0.20-5.50 parts, pH adjuster 0.10-0.35 parts, and the balance is water.

[0030] The oral care composition comprises strontium ions and Rhizoma Drynariae extract in a weight ratio of (0.10-1.75):(0.10-5.00), preferably (0.10-1.75):(0.10-2.00), with the strontium ions accounting for 0.10-1.75 parts by weight (0.10-1.75%) of the oral care product. In the actual preparation process, the strontium ions are added in the form of a strontium salt, and it is sufficient to ensure that the amount of strontium ions added meets the above requirements. If the strontium ions are added in the form of strontium chloride hexahydrate, the weight of strontium chloride hexahydrate is 0.30-5.32 parts (0.30-5.32%), and the ratio of strontium chloride hexahydrate to Rhizoma Drynariae extract is (0.30-5.32):(0.10-5.00).

[0031] The humectant includes at least one of glycerin, sorbitol, polyethylene glycol (PEG), and propylene glycol.

[0032] The abrasive includes at least one of silicon dioxide, calcium bicarbonate and calcium hydrogen phosphate dihydrate.

[0033] The thickener includes at least one of sodium carboxymethyl cellulose, hydroxyethyl cellulose, carbomer, carrageenan, guar gum and xanthan gum.

[0034] The surfactant includes at least one of sodium lauryl sulfate, cocoyl alanine triacetate ammonium, cocamidopropyl betaine, potassium cocoyl glycinate, sodium cocoyl glycinate, sodium lauroyl sarcosinate, alkyl glucoside, sodium laureth sulfate and triethanolamine cocoyl glutamate.

[0035] The sweetener includes at least one of saccharin sodium, aspartame, stevia, sucralose, acesulfame potassium, sucrose and xylitol.

[0036] The flavor includes one of lemon flavor, fruit flavor, spearmint flavor, wintergreen flavor, peppermint and mint flavor oil.

[0037] The pH adjuster includes at least one of tetrasodium pyrophosphate, disodium dihydrogen pyrophosphate, sodium hydroxide, sodium bicarbonate, and sodium tripolyphosphate.

[0038] Except for the composition formed by strontium ions and Drynaria extract, the other ingredients are all ordinary toothpaste ingredients. In the examples and comparative examples, in order to facilitate the demonstration of the technical effects, ordinary toothpaste is used to illustrate the efficacy of the strontium ion and Drynaria extract composition and the preparation method. It should be noted that the strontium ion and Drynaria extract composition is also applicable to other types of toothpaste, such as adding other therapeutic ingredients, anti-caries and anti-sensitivity ingredients, traditional Chinese medicine extract ingredients, whitening ingredients, etc.

[0039] An oral care product containing an acid-resistant oral care composition is prepared by the following method: S1: Preparation of an acid-resistant oral care composition: A soluble strontium salt is mixed and dispersed with water in a formula at a mass ratio of 1:1-1:2 to obtain a strontium ion system. Drynaria extract is dispersed in a moisturizer in a formula at a mass ratio of 1:1-1:3 to obtain a Drynaria system. The strontium ion system and the Drynaria system are mixed and then ultrasonically treated to obtain an acid-resistant, repairing oral care composition. The ultrasonic treatment parameters are: ultrasonic power of 150-250W (preferably 180W) and ultrasonic time of 20-50 minutes (preferably 30 minutes). Conventional ultrasonic equipment has a frequency of 15-25kHz; this solution uses an ultrasonic equipment with an ultrasonic frequency of approximately 20kHz.

[0040] S2: Add a thickener to the moisturizer (the remainder), stir until homogeneous, then add the acid-resistant oral care composition, sweetener, surfactant, pH adjuster and water (the remainder after preparing the acid-resistant oral care composition), and stir evenly.

[0041] S3: adding abrasives to the above mixture, stirring evenly and then vacuuming; finally adding essence, stirring evenly, and degassing, and the oral care product is prepared, specifically toothpaste.

[0042] Example 1 The toothpaste was prepared according to the formula in Table 1. The preparation method is as follows: S1: Preparation of an acid-resistant oral care composition: Strontium chloride hexahydrate is mixed and dispersed with water in a formula at a mass ratio of 1:2 to obtain a strontium ion system. Drynaria extract is dispersed in polyethylene glycol 400 at a mass ratio of 1:2.5 to obtain a drynaria system. The strontium ion system and the drynaria system are mixed and then ultrasonically treated to obtain an acid-resistant, repairing oral care composition. The ultrasonic treatment parameters are: ultrasonic power of 180W and ultrasonic time of 30 minutes. If the amount of polyethylene glycol in the formula is insufficient, the drynaria extract can be mixed with the entire amount of polyethylene glycol, which can also ensure that the drynaria extract is fully dispersed and achieve the desired effect.

[0043] S2: Add thickeners (xanthan gum and carboxymethyl cellulose gum) to the remaining moisturizer (sorbitol and the remaining polyethylene glycol), stir until homogeneous, then add the antacid repair oral care composition, sweetener (saccharin sodium), surfactant (sodium lauryl sulfate), pH adjuster (sodium hydroxide) and water (the remaining amount after preparing the composition preform), and stir evenly.

[0044] S3: add 30% of the mass of the abrasive silica to the mixture, mix and stir until uniform, then add the remaining abrasive silica, stir until uniform, and then vacuum; add the flavoring, mix and stir until uniform, degas, and obtain the toothpaste.

[0045] The formulations of Examples 2-9 and Comparative Examples 1-11 are shown in Tables 1, 2 and 3, and the preparation method is as in Example 1. It should be noted that: In Comparative Examples 1 and 2, no drynaria extract was added, and the preparation method was slightly different in step S1: strontium chloride hexahydrate was mixed with water in the formulation at a mass ratio of 1:2 to obtain a strontium ion system. Then, ultrasonic treatment was performed to obtain the anti-acid repair oral care composition. The parameters of the ultrasonic treatment were: ultrasonic power 180 W, ultrasonic time 30 min. The subsequent processing steps were performed in the manner of Example 1.

[0046] In Comparative Examples 7 and 8, no strontium chloride hexahydrate was added, and the preparation method was slightly different in step S1: the drynaria extract was dispersed in polyethylene glycol 400 at a mass ratio of 1:2.5 to obtain a drynaria system. Then, ultrasonic treatment was performed to obtain the anti-acid repair oral care composition. The parameters of the ultrasonic treatment were: ultrasonic power 180 W, ultrasonic time 30 min. The subsequent processing steps were performed in the manner of Example 1.

[0047] In Comparative Example 9, no drynaria extract and no strontium chloride hexahydrate were added, so step S1 was omitted, and the toothpaste was obtained as follows: the humectants (sorbitol and polyethylene glycol) were mixed with the thickening agents (xanthan gum and carboxymethyl cellulose gum), and stirred until uniform, then the anti-acid repair oral care composition, the sweetener (sodium saccharin), the surfactant (sodium lauryl sulfate), the pH adjuster (sodium hydroxide), and water (the remaining amount after preparing the composition pre-product) were added and stirred until uniform. 30% of the mass of the abrasive silica was added to the mixture, mixed and stirred until uniform, then the remaining abrasive silica was added, stirred until uniform, and then vacuumed; the flavoring was added, mixed and stirred until uniform, degassed, and the toothpaste was obtained.

[0048] In Comparative Example 10, the Drynaria extract was replaced with pine bark extract. More specifically, the pine bark extract was purchased commercially. The main component of the pine bark extract is proanthocyanidins, with a purity of approximately 95% (i.e., the pine bark extract contains approximately 95% proanthocyanidins). Among the proanthocyanidins, the content of oligomeric proanthocyanidins is approximately 84%. Proanthocyanidins is a general term for a large class of polyphenolic compounds found widely in plants. Their common characteristic is that they all produce anthocyanidins upon heating in acidic media, hence the term proanthocyanidins. Proanthocyanidins are a type of pigment found in plants and are widely present in various plants. The simplest proanthocyanidins are catechin, epicatechin, or dimers of catechin and epicatechin. Other proanthocyanidins include trimers, tetramers, and even decamers. Based on the degree of polymerization, dimers to pentamers are referred to as oligomeric proanthocyanidins (OPCs), while pentamers and above are referred to as polymeric proanthocyanidins (PPCs).

[0049] The formula of Comparative Example 11 is the same as that of Example 6, but the preparation method of step S1 is different, specifically: Strontium chloride hexahydrate and water in the formula were mixed and dispersed in a mass ratio of 1:2 to obtain a strontium ion system. Drynaria extract was dispersed in polyethylene glycol 400 in a mass ratio of 1:2.5 to obtain a drynaria system. The drynaria system was slowly added (30 drops / minute) to the strontium ion system at 200 rpm while stirring, followed by stirring for 30 minutes to prepare an acid-resistant oral care composition. The subsequent preparation process was the same as in Example 1. The strontium ion system and drynaria system were mixed dropwise, following the preparation method described in a prior patent.

[0050] The specific situation is: Table 1: Toothpaste formula of the embodiment (unit: part; total number of parts: 100 parts)

[0051] Table 2: Toothpaste formulas of Comparative Examples 1-6 (unit: parts; total parts: 100 parts)

[0052] Table 3: Toothpaste formula of comparative examples 7-11 (unit: part; total number of parts: 100 parts)

[0053] Experimental Example 1: Evaluation of the ability to repair the surface of tooth hard tissue Freshly extracted bovine incisors were cut and polished to produce dentin blocks of approximately 6 mm × 6 mm × 2 mm in size. These blocks were then polished on a grinding and polishing machine using 320#, 800#, 3000#, and 5000# silicon carbide water-sandpaper in sequence until the surface was smooth and flat. The dentin blocks were then inverted and embedded in a denture base resin in a dental mold. After solidification, the blocks were demolded, and the dentin surface was ground to be on the same surface as the resin. Finally, a windowed polyester tape was used to cover the surface of the tooth sample to create a test area of ​​approximately 3 × 6 mm in size. 2 .

[0054] A certain weight of test sample (toothpaste prepared in the Examples and Comparative Examples) and deionized water were weighed at a ratio of 1:3 (test sample:water). The toothpaste was dispersed by stirring with a glass rod and then homogenized with a magnetic stirrer to prepare a "toothpaste slurry." The experimental dentin samples were immersed in 100 ml of artificial saliva for 45 minutes, mineralized in 100 ml of "toothpaste slurry" for 45 minutes, rinsed with deionized water, and then treated with 100 ml of artificial saliva for 45 minutes. A contact profilometer was used to measure the average depth (i.e., mineralized layer thickness) of the exposed dentin surface (test area) of each sample before and after "toothpaste slurry" treatment. The data were recorded. The experiment was repeated three times for each toothpaste sample. The thickness of the mineralized layer on the dentin surface after "toothpaste slurry" treatment was then compared. A thicker mineralized layer indicates a stronger repair capability. Detailed experimental data are shown in Table 4.

[0055] Table 4: Evaluation results of the ability to repair the surface of the hard tissue of the tooth essence (the experimental results are the average of three repeated experiments)

[0056] The experimental data in Table 4 are analyzed as follows: (1) Drynaria extract enhances the effect of strontium salt-induced dentin mineralization In the presence of Drynaria extract, increasing the amount of strontium salt significantly increased the thickness of the mineralized protective layer formed on the surface of the dentin. Specifically, comparing Example 1 and Example 4 (where the Drynaria extract dosage was the same at 0.1 part and strontium chloride hexahydrate was increased from 0.30 part to 5.32 parts), the thickness of the mineralized layer increased by 1.14 μm, from 0.93 μm to 2.07 μm. Similarly, in Examples 2 and 5, where the Drynaria extract dosage was the same at 0.5 part, increasing the amount of strontium chloride hexahydrate increased the thickness of the mineralized layer from 1.24 μm to 2.65 μm, a 1.41 μm increase. In Examples 3 and 6, where the Drynaria extract dosage was 2 parts, the thickness of the mineralized layer increased by 2.38 μm, from 2.16 μm to 4.54 μm.

[0057] It is worth noting that as the amount of Drynaria extract increases, the growth value of the mineralized layer thickness also shows a clear increasing trend (1.14μm→1.41μm→2.38μm). However, without the addition of Drynaria extract, even if the amount of strontium chloride hexahydrate increases from 0.30 parts to 5.32 parts, the thickness of the mineralized layer only increases from 0.61μm to 1.43μm, an increase of 0.82μm (Comparative Examples 1 and 2). Although Drynaria extract has basically no effect on promoting the mineralization of the dentin surface when used alone (as shown in Comparative Examples 7 and 8), when it is used in combination with strontium salts, it can significantly enhance the effect of strontium salts and effectively promote the mineralization process of dentin, reflecting the synergistic effect between the two.

[0058] (2) Synergistic effect of combined use of Drynaria extract and strontium salt on increasing the thickness of the tooth mineral layer When the two ingredients are used together, their effect not only exceeds that of either ingredient alone, but also exceeds the sum of the effects of both individually (i.e., "combined effect > effect of A alone + effect of B alone"). The thickness of the mineralized layer directly reflects the ability to promote mineralization; the thicker the layer, the stronger the effect.

[0059] In Example 1 (0.3 parts strontium chloride hexahydrate + 0.1 parts Drynaria extract), the combined use of strontium chloride hexahydrate and Drynaria extract resulted in a mineralized layer thickness of 0.93 μm. Using strontium chloride hexahydrate alone (Comparative Example 1: 0.3 parts strontium chloride hexahydrate) resulted in a mineralized layer thickness of 0.61 μm; using Drynaria extract alone (Comparative Example 7: 0.1 parts Drynaria extract) resulted in a mineralized layer thickness of 0.01 μm. The sum of the individual effects: 0.61 + 0.01 = 0.62 μm. This indicates that the combined effect exceeds the sum of the individual effects (0.93 > 0.62), exceeding 50%. Therefore, the combined use of strontium chloride hexahydrate and Drynaria extract demonstrates a synergistic effect in increasing mineralized layer thickness.

[0060] Similarly, Example 6 (5.32 parts of strontium chloride hexahydrate, 2 parts of Drynaria extract; mineralized layer thickness 4.54 μm), Comparative Example 2 (5.32 parts of strontium chloride hexahydrate; mineralized layer thickness 1.43 μm), Comparative Example 8 (2 parts of Drynaria extract; mineralized layer thickness 0.14 μm) were analyzed; Example 3 (0.3 parts of strontium chloride hexahydrate, 2 parts of Drynaria extract; mineralized layer thickness 2.16 μm), Comparative Example 1 (0.3 parts of strontium chloride hexahydrate; mineralized layer thickness 0.61 μm), Comparative Example Analysis of Example 8 (2 parts of Drynaria extract; mineralized layer thickness 0.14 μm); analysis of Example 4 (5.32 parts of strontium chloride hexahydrate, 0.1 part of Drynaria extract; mineralized layer thickness 2.07 μm), Comparative Example 2 (5.32 parts of strontium chloride hexahydrate; mineralized layer thickness 1.43 μm), and Comparative Example 7 (0.1 part of Drynaria extract; mineralized layer thickness 0.01 μm) revealed varying degrees of synergistic synergy between strontium chloride hexahydrate and Drynaria extract in increasing mineralized layer thickness. In all examples, the combined mineralized layer thickness achieved was significantly greater than that achieved with Drynaria extract alone (which had an effect of only 0.01-0.14 μm, almost insignificant); significantly greater than that achieved with strontium chloride alone (increases by 45%-254%); and greater than the combined effects of both components alone (meeting the synergistic characteristic of "1+1>2").

[0061] In summary, strontium chloride hexahydrate and Drynaria extract have a clear and significant synergistic effect in promoting the formation of mineralized layer (related to dentin repair), and appropriately increasing the dosage of Drynaria extract (within the experimental range) can enhance the synergistic effect.

[0062] (3) Effect of the dosage of Drynaria fortunei extract on the effect of strontium salt When the amount of Drynaria extract was lower than that in the examples, the thickness of the mineralized layer decreased significantly, indicating that the amount of Drynaria extract was the key limiting factor for synergistic effect, and insufficient amount would significantly weaken the effect. When strontium chloride hexahydrate is 0.3 parts: compared with Example 1 (0.1 parts of Drynaria rhizome, mineralized layer 0.93 μm) and Comparative Example 3 (0.05 parts of Drynaria rhizome, mineralized layer 0.67 μm), after the dosage is halved, the thickness of the mineralized layer decreases by about 29% (0.93→0.67).

[0063] When strontium chloride hexahydrate is 5.32 parts: compared with Example 4 (0.1 parts of Drynaria rhizome, mineralized layer 2.07 μm) and Comparative Example 5 (0.05 parts of Drynaria rhizome, mineralized layer 1.44 μm), after the dosage is halved, the thickness of the mineralized layer decreases by about 31.0% (2.07→1.44).

[0064] This result indicates that at a certain strontium chloride concentration, when the dosage of Drynaria fortunei extract is lower than a certain threshold, its synergistic effect with strontium chloride will be significantly weakened, and the extent of the dosage reduction is positively correlated with the extent of the decrease in the mineralized layer thickness.

[0065] When the dosage of Drynaria extract is higher than that in the example, the thickness of the mineralized layer increases only slightly, indicating that the dosage of Drynaria extract has approached the "saturation point" and further increasing the dosage will have limited effect on the synergistic effect. When strontium chloride hexahydrate is 0.3 parts: compared with Example 3 (2 parts of Drynaria rhizome, mineralized layer 2.16 μm) and Comparative Example 4 (2.5 parts of Drynaria rhizome, mineralized layer 2.23 μm), after the dosage is increased by 25% (2 → 2.5 parts), the thickness of the mineralized layer only increases by about 3% (2.16 → 2.23).

[0066] When strontium chloride hexahydrate is 5.32 parts: compared with Example 6 (2 parts of Drynaria rhizome, mineralized layer 4.54 μm) and Comparative Example 6 (2.5 parts of Drynaria rhizome, mineralized layer 4.68 μm), after the dosage is increased by 25% (2 → 2.5 parts), the thickness of the mineralized layer only increases by about 3% (4.54 → 4.68).

[0067] This result shows that when the dosage of Drynaria fortunei extract exceeds the dosage in the example, its synergistic effect with strontium chloride enters a "plateau period", and the increase in dosage on the thickness of the mineralized layer is much smaller than the increase in dosage, that is, there is a "diminishing marginal benefits" phenomenon.

[0068] Combined with the data, it can be seen that under the dosage of strontium chloride hexahydrate involved in the experiment (0.3-5.32), there is a more optimal synergistic dosage range (0.1-2) for Drynaria fortunei extract: when the dosage is lower than this range (such as 0.05 parts, lower than 0.1 parts in the embodiment), the synergistic effect is significantly weakened and the thickness of the mineralized layer decreases significantly; when the dosage is in this range (such as 0.1-2 parts), the synergistic effect is fully exerted and the thickness of the mineralized layer reaches a higher level; when the dosage is higher than this range (such as 2.5 parts, higher than 2 parts in the embodiment), the synergistic effect is limited, the thickness of the mineralized layer only increases slightly, and the practical significance of continuing to increase the dosage is relatively low.

[0069] In summary, the synergistic effect of strontium chloride hexahydrate and Drynaria fortunei extract is not simply "the higher the dosage, the better the effect", but requires the dosage of the two to be matched within a reasonable range to maximize the mineralization promotion effect.

[0070] (4) Advantages of Drynaria fortunei extract over other plant extracts Comparative Example 10, which combined pine bark extract with strontium chloride hexahydrate, showed less effective results in promoting mineralization compared to Example 1, with the thickness of the mineralized layer decreasing by approximately 25%. This indicates that Drynaria extract outperformed pine bark extract in enhancing the acid-resistant repair effect, making it a more superior synergistic ingredient.

[0071] (5) Influence of preparation process on the effect of oral care products In Comparative Example 11, strontium chloride hexahydrate and Drynaria extract were prepared differently: the Drynaria system was slowly added dropwise to the strontium ion system. Compared with Example 6, the thickness of the mineralized layer decreased from 4.54 to 3.42 (a decrease of approximately 25%). This demonstrates that the preparation process plays a crucial role in the synergistic effect of strontium chloride hexahydrate and Drynaria extract.

[0072] Experimental Example 2: Evaluation of the ability to resist acid erosion on the surface of tooth hard tissue A certain weight of test sample and deionized water were weighed at a ratio of 1:3 (test sample:water). The toothpaste was dispersed by stirring with a glass rod and then homogenized with a magnetic stirrer to obtain a "toothpaste slurry." The experimental dentin samples were immersed in 100 ml of artificial saliva for 45 minutes, mineralized in 100 ml of "toothpaste slurry" for 45 minutes, rinsed with deionized water, and treated with 100 ml of artificial saliva for 45 minutes. The samples were then etched with 100 ml of 1% citric acid solution for 240 minutes. The samples were then rinsed with deionized water and immersed in 100 ml of artificial saliva for 60 minutes. The depth of the exposed dentin surface profile change was measured using a contact profilometer and recorded. The etch depth of the artificial saliva-treated samples (artificial saliva group) was used as a control to calculate the depth of acid etch resistance loss. A greater depth of acid etch resistance loss indicates a stronger resistance of the mineralized layer in the experimental group and a greater ability to repair acid etch. Acid erosion resistance (μm) = Acid erosion depth in the artificial saliva group (μm) minus Acid erosion depth in the test group (μm). The artificial saliva group refers to the process of "mineralizing in 100 ml of toothpaste slurry for 60 minutes" instead of "immersing in 100 ml of artificial saliva for 60 minutes." See Table 5 for detailed experimental data.

[0073] Table 5: Data on the acid erosion resistance of tooth hard tissue (the experimental results are the average of three repeated experiments)

[0074] The experimental data in Table 5 are analyzed as follows: (1) Effect of the dosage of Drynaria fortunei extract At a fixed strontium chloride hexahydrate dosage (0.30 parts for Examples 1-3 and 5.32 parts for Examples 4-6), increasing the Drynaria extract dosage from 0.1 to 2 parts significantly improved the acid etch resistance. In the 0.30 part strontium chloride hexahydrate group, the acid etch resistance changed from 2.31 μm to 6.45 μm to 10.73 μm (an increase of approximately 352%); in the 5.32 part strontium chloride group, the acid etch resistance changed from 12.31 μm to 15.43 μm to 26.14 μm (an increase of approximately 112%). This indicates that the dosage of Drynaria extract is positively correlated with the acid etch resistance, and the synergistic effect of Drynaria extract is even more pronounced at higher strontium chloride dosages (reaching a maximum of 26.14 μm in Example 6).

[0075] (2) Effect of the dosage of strontium chloride hexahydrate Comparing the effects of different strontium chlorides at the same dosage of Drynaria Rhizoma, when using 0.1 parts of Drynaria Rhizoma extract, the group of 0.30 parts of strontium chloride hexahydrate (Example 1: 2.31) is less than the group of 5.32 parts of strontium chloride hexahydrate (Example 4: 12.31, an increase of about 433%); when using 2 parts of Drynaria Rhizoma: the group of 0.30 parts of strontium chloride hexahydrate (Example 3: 10.73) is less than the group of 5.32 parts of strontium chloride hexahydrate (Example 6: 26.14, an increase of about 143%).

[0076] It can be seen that increasing the dosage of strontium chloride hexahydrate can significantly enhance the anti-acid corrosion performance, and has a synergistic effect with the drynaria extract.

[0077] (3) Strontium chloride hexahydrate and Drynaria extract synergistically increase the product's anti-acid corrosion performance The synergistic effect analysis of Example 4, Comparative Example 2 and Comparative Example 7 is as follows: Effect of single ingredient: When strontium chloride hexahydrate acts alone (Comparative Example 2), the effect is significant (7.65 μm), but when Drynaria fortunei extract acts alone (Comparative Example 7), the effect is extremely weak (0.12 μm).

[0078] Combined effect: In Example 4, after the two are combined, the acid corrosion resistance (12.31 μm) is much higher than that of single strontium chloride hexahydrate (7.65 μm), and far exceeds the theoretical superposition value of "the effect of strontium chloride alone + the effect of Drynaria fortunei alone" (7.65+0.12=7.77 μm).

[0079] It can be seen that strontium chloride hexahydrate and Drynaria extract have obvious synergistic effect at this formula ratio. Drynaria extract can enhance the anti-acid erosion effect of high-dose strontium chloride. The effect of combined use of the two is far better than that of a single ingredient.

[0080] The synergistic effect analysis of Example 1, Comparative Example 1 and Comparative Example 7 is as follows: Effect of single ingredient: Low-dose strontium chloride (Comparative Example 1) had a weak effect (0.31 μm) when acting alone, and Drynaria fortunei extract had an extremely weak effect (0.12 μm) when acting alone (Comparative Example 7). The theoretical superposition value of the two alone was only 0.43 μm (0.31+0.12).

[0081] Combined use effect: After the two are combined in Example 1, the acid corrosion resistance strength (2.31 μm) is significantly higher than the effect of a single component and the theoretical superposition value, which is 5.37 times the superposition value (2.31÷0.43≈5.37).

[0082] It can be seen that when low-dose strontium chloride is used in combination with Drynaria fortunei extract, it shows a very strong synergistic effect. The combination of the two can greatly enhance the anti-acid erosion effect, which is far beyond the comparison of the simple superposition of a single ingredient.

[0083] Whether it is high-dose strontium chloride (Example 4) or low-dose strontium chloride (Example 1), when used in combination with Drynaria fortunei extract, its acid corrosion resistance is significantly higher than the effect of the two ingredients acting alone and the theoretical superposition value, which clearly proves that strontium chloride hexahydrate and Drynaria fortunei extract have a significant synergistic effect in acid corrosion resistance, and this synergistic effect can be manifested at different strontium chloride doses.

[0084] Experimental Example 3: Paste Stability Test The pastes of the examples and comparative examples were packaged as conventional finished toothpastes. The stability of the examples and comparative examples was observed at room temperature and 45° C. The experimental results are shown in Table 6.

[0085] Table 6: Observation results of paste stability (the left side of “ / ” indicates the test results at room temperature, and the right side indicates the test results at 45°C; if the test results are the same in both cases, they will not be recorded repeatedly)

[0086] It can be seen from the experimental results in Table 6 that the use of strontium salts and Rhizoma Drynariae extract to prepare toothpaste is the first attempt of this technical solution. The addition method of strontium salts and Rhizoma Drynariae extract has a very significant effect on the color and stability of the paste, requiring special pretreatment. This technical solution requires that strontium salts and Rhizoma Drynariae extract be prepared into a preform, and the solvent for dispersing the Rhizoma Drynariae extract needs to adopt the polar liquid in the formula (for example, glycerol, PEG, propylene glycol and other wetting agents) and be prepared under a certain ultrasonic process. Comparative Example 11 does not adopt the toothpaste preparation process of this solution (does not adopt ultrasonic process), resulting in a significant negative impact on the appearance and stability of the paste, especially the thermal stability (discoloration occurs). Rhizoma Drynariae extract needs to be mixed with wetting agents such as glycerol, PEG, propylene glycol and a strontium salt aqueous solution, and the preform formed after ultrasonic dispersion and action is used for the preparation of toothpaste paste, so that discoloration can be effectively prevented under subsequent high temperature conditions. In Comparative Examples 4 and 6, although an ultrasonic pre-preparation process was used in the high-proportion Drynaria extract, due to the high content of the Drynaria extract, when stored at a relatively high temperature for a long time, in addition to discoloration, there was even an undesirable phenomenon of material agglomeration (manifested as coarsening) and water-oil separation (water separation).

[0087] The above is only an embodiment of the present invention, and the common knowledge such as the specific technical solutions and / or characteristics in the solution are not described in detail here. It should be pointed out that for those skilled in the art, without departing from the technical solution of the present invention, several variations and improvements can be made, which should also be regarded as the scope of protection of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the description can be used to interpret the content of the claims.

Claims

1. A composition containing a Rhizoma Drynariae extract for enhancing the acid-resistant repair effect, characterized in that: Includes strontium ions and drynaria extract.

2. The composition for enhancing the anti-acid repair effect containing the Drynaria Rhizoma extract according to claim 1, characterized in that: The mass ratio of strontium ion to drynaria extract is (0.10-1.75): (0.10-5.00); preferably, the mass ratio of strontium ion to drynaria extract is (0.10-1.75): (0.10-2.00).

3. The composition for enhancing the anti-acid repair effect containing the Drynaria Rhizoma extract according to claim 2, characterized in that: The content of naringin in the drynaria extract is ≥20%.

4. The composition comprising the extract of Drynaria fortunei for enhancing the anti-acid repair effect according to claim 3, characterized in that: The strontium ions are provided in the form of soluble strontium salts; the soluble strontium salts include at least one of hydrates and non-hydrates of strontium acetate, strontium chloride, strontium nitrate, strontium lactate, and strontium bromide.

5. An oral care product comprising a composition for enhancing the acid resistance and repairing effect of a Rhizoma Drynariae extract according to any one of claims 1 to 4, characterized in that: The mass ratio of strontium ions in the oral care products is 0.10-1.75%, and the mass ratio of drynaria extract in the oral care products is 0.10-2.00%.

6. The oral care product according to claim 5, characterized in that: The oral care product further comprises the following raw materials in parts by weight: Moisturizer 15.00-65.00 parts, abrasive 0.00-55.00 parts, thickener 0.20-9.00 parts, surfactant 1.00-22.00 parts, sweetener 0.20-3.00 parts, flavor 0.20-5.50 parts, pH adjuster 0.10-0.35 parts.

7. The oral care product according to claim 6, characterized in that: The moisturizing agent includes at least one of glycerin, sorbitol, polyethylene glycol (PEG) and propylene glycol; The friction agent includes at least one of silicon dioxide, calcium bicarbonate and calcium hydrogen phosphate dihydrate; The thickener comprises at least one of sodium carboxymethyl cellulose, hydroxyethyl cellulose, carbomer, carrageenan, guar gum and xanthan gum; The surfactant comprises at least one of sodium lauryl sulfate, cocoyl alanine triacetate ammonium, cocamidopropyl betaine, potassium cocoyl glycinate, sodium cocoyl glycinate, sodium lauroyl sarcosinate, alkyl glucoside, sodium laureth sulfate and triethanolamine cocoyl glutamate; The sweetener comprises at least one of saccharin sodium, aspartame, stevia, sucralose, acesulfame potassium, sucrose and xylitol; The flavor comprises one of lemon flavor, fruit flavor, spearmint flavor, wintergreen flavor, peppermint and mint essential oil; The pH adjuster includes at least one of tetrasodium pyrophosphate, disodium dihydrogen pyrophosphate, sodium hydroxide, sodium bicarbonate and sodium tripolyphosphate.

8. The oral care product according to claim 7, characterized in that: The acid-resistant oral care composition is prepared by the following method: A soluble strontium salt is mixed with water in a mass ratio of 1:1-1:2 to obtain a strontium ion system; a drynaria extract is mixed with a moisturizer in a mass ratio of 1:1-1:3 to obtain a drynaria system; the strontium ion system and the drynaria system are mixed and then ultrasonically treated to obtain an acid-resistant repairing oral care composition; the parameters of the ultrasonic treatment are: ultrasonic power 150-250W, ultrasonic time 20-50min.

9. The method for preparing the oral care product according to claim 8, wherein: The method includes the following steps: S1: Soluble strontium salt and water are mixed in a mass ratio of 1:1-1:2 to obtain a strontium ion system; Mixing the drynaria extract and polyethylene glycol at a mass ratio of 1:1-1:3 to obtain a drynaria system; The strontium ion system and the drynaria system are mixed, and then ultrasonically treated to obtain an acid-resistant and repairing oral care composition; S2: sorbitol and the remaining polyethylene glycol are mixed, and a thickener is added and mixed evenly, and then the acid-resistant oral care composition, sweetener, surfactant, pH regulator and the remaining water are added and stirred evenly. S3: Add the friction agent, stir evenly and then evacuate; finally add the essence, stir evenly and degas.

10. The method for preparing the oral care product according to claim 9, characterized in that: The soluble strontium salt is strontium chloride hexahydrate; the mass ratio of strontium chloride hexahydrate to drynaria extract is (0.30-5.32): (0.10-5.00); preferably, the mass ratio of strontium chloride hexahydrate to drynaria extract is (0.30-5.32): (0.10-2.00); The parameters of the ultrasonic treatment are: ultrasonic power 150-250W, ultrasonic time 20-50min; preferably, the ultrasonic power is 180W; and the ultrasonic time is 30min.

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