Microneedle-containing coptis toothpaste and preparation method thereof

Abstract

The invention discloses rhizoma coptidis toothpaste containing microneedles. The rhizoma coptidis toothpaste is prepared from the following components in parts by weight: 40 to 50 parts of a humectant, 20 to 30 parts of a friction agent, 1 to 2 parts of a thickening agent, 3 to 4 parts of a foaming agent, 0.1 to 0.3 part of a sweetening agent, 0.1 to 1 part of a rhizoma coptidis extract, 0.1 to 1 part of sponge spicules, 0.2 to 0.6 part of menthol, 0.2 to 0.6 part of peppermint oil, 0.1 to 0.6 part of fruit essence, 0.1 to 0.2 part of a preservative and 20 to 30 parts of ultrapure water, wherein the coptis chinensis extract is a 70% ethanol extract of coptis chinensis. The natural sponge spicule is introduced into a traditional Chinese medicine toothpaste system for the first time, adsorption slow release and physical cleaning effects generated by a porous structure of the natural sponge spicule are utilized to cooperate with heat clearing and fire purging effects of traditional coptis chinensis, and the toothpaste has the effects of cleaning teeth, relieving gingival discomfort and relieving oral cavity internal heat.

Description

Technical Field

[0001] This invention belongs to the field of oral care products, specifically relating to a Coptis chinensis toothpaste containing microneedles and its preparation method. Background Technology

[0002] Toothpaste, as an essential daily oral hygiene product, has evolved from simply cleaning teeth to preventing and treating specific oral problems. Traditional Chinese medicine, due to its natural properties and multi-target effects, is widely used in functional toothpastes. Coptis chinensis, a commonly used traditional Chinese medicine, has the effects of clearing heat and drying dampness, purging fire and detoxifying, showing potential in relieving gum problems and oral inflammation. However, the oral environment is moist and subject to significant dynamic changes, limiting the residence time of the effective components of traditional Chinese medicine in the mouth. Furthermore, the presence of physiological barriers on the oral mucosa and tooth surface restricts the efficiency of the active ingredients to some extent.

[0003] Currently, micron-sized silica materials (such as silica and hydrated silica) or calcareous materials (such as dicalcium phosphate) are typically added to toothpaste as abrasives for mechanical cleaning, achieving both physical cleaning and polishing effects. These materials are mostly dense or non-directionally porous, and their cleaning effect is balanced with enamel abrasion primarily by controlling hardness, particle size, and morphology. They do not possess the function of acting as carriers for active ingredients or forming temporary microchannels on the oral mucosa surface to promote the penetration of effective ingredients.

[0004] Therefore, existing Chinese herbal toothpastes still mainly rely on the effects of the active ingredients themselves to exert the efficacy of the Chinese herbal active ingredients. They lack effective delivery methods for the complex oral environment, making it difficult to achieve a synergistic enhancement of physical cleaning and the efficient effect of active ingredients. There is still room for further improvement in related technologies. Summary of the Invention

[0005] The purpose of this invention is to address the shortcomings of existing Coptis chinensis toothpaste in terms of poor penetration and absorption of active ingredients, and to provide a Coptis chinensis toothpaste containing microneedles. This toothpaste can significantly improve the penetration and absorption efficiency of Coptis chinensis active ingredients in the oral cavity, enhance its antibacterial and anti-inflammatory effects, improve oral problems, and also clean teeth, relieve gum discomfort, and reduce oral inflammation.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A toothpaste containing microneedles made from the following components in parts by weight: 40-50 parts humectant, 20-30 parts abrasive, 1-2 parts thickener, 3-4 parts foaming agent, 0.1-0.3 parts sweetener, 0.1-1 part Coptis chinensis extract, 0.1-1 part sponge needles, 0.2-0.6 parts menthol, 0.2-0.6 parts peppermint oil, 0.1-0.6 parts fruit flavoring, 0.1-0.2 parts preservative, and 20-30 parts ultrapure water; wherein the Coptis chinensis extract is a 70% ethanol extract of Coptis chinensis.

[0008] Preferably, the Coptis chinensis toothpaste containing microneedles is made from the following components in parts by weight: 40-45 parts of moisturizer, 21-22 parts of abrasive, 1-2 parts of thickener, 3-3.6 parts of foaming agent, 0.1-0.3 parts of sweetener, 0.1-1 parts of Coptis chinensis extract, 0.1-1 parts of sponge spicules, 0.2-0.6 parts of menthol, 0.2-0.6 parts of peppermint oil, 0.1-0.6 parts of fruit flavoring, 0.1-0.2 parts of preservative, and 20-30 parts of ultrapure water.

[0009] The Coptis chinensis extract is obtained by crushing Coptis chinensis, passing it through a 120-mesh sieve, and extracting it twice by reflux with 70% ethanol as the extraction solvent, each extraction lasting 1 hour. The extract is then filtered, the filtrate is concentrated under reduced pressure, and dried under vacuum. The material-to-liquid ratio for each extraction is 1:10 g / mL.

[0010] The sponge bone needles are porous silica bone needles with an average length of 200-300 μm and an average diameter of 15-20 μm.

[0011] The moisturizer is at least one of sorbitol and glycerin.

[0012] Preferably, the moisturizer is a combination of sorbitol and glycerin in a weight ratio of 5:1 to 6:1.

[0013] More preferably, the moisturizer is a combination of sorbitol and glycerin in a weight ratio of 5:1.

[0014] The friction agent is at least one of hydrated silica, silicon dioxide, and dicalcium phosphate.

[0015] Preferably, the friction agent is a combination of hydrated silica and silicon dioxide in a weight ratio of 1.8:1 to 2.2:1.

[0016] More preferably, the friction agent is a combination of hydrated silica and silicon dioxide in a weight ratio of 2:1 to 2.2:1.

[0017] The silicon dioxide mentioned is thickened silicon dioxide.

[0018] The thickener is at least one of sodium carboxymethyl cellulose (CMC-Na), carrageenan, and xanthan gum.

[0019] Preferably, the thickener is a combination of sodium carboxymethyl cellulose and xanthan gum in a weight ratio of 6.5:1.

[0020] The foaming agent is at least one of sodium lauryl sulfate, sodium lauroyl sarcosinate, and cocamidopropyl betaine.

[0021] Preferably, the foaming agent is a combination of sodium lauryl sulfate and cocamidopropyl betaine in a weight ratio of 1:0.8 to 1:1.

[0022] More preferably, the foaming agent is a combination of sodium lauryl sulfate and cocamidopropyl betaine in a weight ratio of 1:0.8.

[0023] The sweetener mentioned is sucralose.

[0024] The fruit flavoring is at least one of lemon flavoring and peach flavoring.

[0025] The preservative mentioned is sodium benzoate.

[0026] More preferably, the Coptis chinensis toothpaste containing microneedles is made from the following components in parts by weight: 35 parts sorbitol, 7 parts glycerin, 14 parts hydrated silica, 7 parts thickening silica, 1.3 parts sodium carboxymethyl cellulose, 0.2 parts xanthan gum, 2 parts sodium lauryl sulfate, 1.6 parts cocamidopropyl betaine, 1 part sponge needles, 0.3 parts menthol, 0.2 parts peppermint oil, 0.5 parts lemon flavor, 0.1 parts sodium benzoate, 0.1 parts sucralose, 0.1 parts Coptis chinensis extract, and 29.6 parts ultrapure water.

[0027] Another object of the present invention is to provide a method for preparing the Coptis chinensis toothpaste containing microneedles, comprising the following steps:

[0028] Step 1: Dissolve the sweetener, preservative, and Coptis chinensis extract in ultrapure water to obtain solution A;

[0029] Step 2: Add the thickener to the humectant and stir at 70-80℃ until evenly mixed to obtain solution B. Stirring at 70-80℃ allows the thickener to be fully wetted, swollen and evenly dispersed, avoiding the formation of agglomerated particles and quickly forming a stable and uniform colloidal system. At the same time, this temperature is relatively mild and will not damage active ingredients such as Coptis chinensis extract, ensuring the toothpaste's fineness, stability and efficacy.

[0030] Step 3: While stirring, add solution A to solution B, stir quickly until the mixture is uniform, and then homogenize until there are no particles to obtain substance C;

[0031] Step 4: Add the abrasive and foaming agent to substance C and stir until evenly mixed. Add the sponge needles and stir evenly. Finally, add menthol, fruit flavoring, and peppermint oil, and continue stirring until stringy. Deaerate to obtain Coptis chinensis toothpaste containing microneedles.

[0032] Step 5: Filling and sealing to obtain the finished toothpaste.

[0033] In step one, the stirring speed is 500-800 rpm.

[0034] The stirring can be done using a magnetic stirrer.

[0035] In step two, preferably, the humectant and thickener are mixed evenly, and then the evenly mixed thickener is added to the evenly mixed humectant. The mixture is stirred at 70-80°C until homogeneous, yielding solution B. This invention premixes the humectant and thickener separately before final mixing, allowing the thickener to fully wet and swell, preventing agglomeration and resulting in a uniform and stable colloidal system. Simultaneously, it ensures the homogeneity of the humectant system, improving the toothpaste's fineness, viscosity stability, and production reproducibility. This provides a reliable matrix for the stable addition and uniform dispersion of active ingredients such as Coptis chinensis extract, enhancing the overall quality and efficacy stability of the toothpaste.

[0036] The stirring speed is 500-800 rpm.

[0037] The stirring can be done using a magnetic stirrer.

[0038] In step three, the speed of rapid stirring is 1000-1200 rpm.

[0039] The rapid stirring described can be achieved using a magnetic stirrer.

[0040] The homogenization was performed using probe-type ultrasound with an ultrasound power of 500 W, an ultrasound frequency of 20 kHz, a homogenization time of 3 min (pulse mode 1:2), and a homogenization temperature of 25℃.

[0041] In step four, preferably, the friction agent and foaming agent are added to substance C and stirred at a speed of 1000-1200 rpm until they are evenly mixed.

[0042] Preferably, after adding the sponge needles, to prevent the sponge needles from breaking during the stirring process, the mixture is slowly stirred at 100-120 rpm until homogeneous.

[0043] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0044] (1) This invention introduces purified and screened natural sponge bone needles into the Coptis chinensis extract toothpaste system for the first time. The sponge bone needles have a hollow drug-carrying structure and a silica micron-scale structure with sharp spikes. They can not only stably load the effective components of Coptis chinensis extract through the hollow structure, but also, under the mechanical action of brushing, accurately form micro-scale channels in target areas such as oral mucosa and gingival sulcus with the sharp spikes. This significantly shortens the diffusion path of the effective components and reduces the permeation barrier resistance formed by the oral mucosa and the tight junction of the epithelium. At the same time, the effective components are released at close range around the microchannels, which can quickly establish a local concentration gradient in the target area and promote the efficient penetration of the effective components into the deep layers of the oral mucosa and the gaps between teeth. This solves the problem of short residence time, slow diffusion and insufficient retention of the effective components of Coptis chinensis extract due to high polarity, oral fluid flushing and physical barrier barriers. It can also reduce the non-specific adsorption of the effective components to toothpaste excipients and improve the availability of the effective components in the system.

[0045] (2) This invention, through the structural advantages of sponge bone needles and the synergistic effect of Coptis chinensis extract, significantly improves the bioavailability and efficacy of its active ingredients in the oral target area without increasing the dosage of Coptis chinensis. It effectively balances the contradiction between enhanced efficacy and safety and mild taste, overcomes the technical difficulty of masking bitterness and promoting penetration in traditional Chinese medicine toothpaste, and makes the product have both excellent oral care efficacy and good user experience. It fills the technical gap in the synergistic application of natural sponge bone needles and Coptis chinensis extract in the field of oral care, and has outstanding innovation and practical application value.

[0046] (3) The toothpaste formula of this invention is scientifically designed, with each component working synergistically to ensure excellent cleaning and foaming performance while also possessing strong antibacterial and anti-inflammatory effects, achieving comprehensive care for teeth and gum tissue. Addressing the technical challenges of shear resistance, fracture prevention, and sedimentation prevention after introducing sponge needles, this invention provides a systematic solution through precise formulation of excipients: using low-adsorption, controllable particle size silica as an abrasive to balance cleaning power and needle structure protection; employing a thickening system of sodium carboxymethyl cellulose and xanthan gum to regulate rheological properties and achieve a balance between uniform needle suspension, shear-induced drug release, and retention after brushing; and using a foaming system primarily composed of mild surfactants to ensure both cleaning and gentleness while avoiding component loss. The synergistic effect of each excipient, sponge needle, and Coptis chinensis extract optimizes the overall performance of the toothpaste from multiple dimensions, including stability, usability, and efficacy, ensuring the full utilization of the core component's advantages. Attached Figure Description

[0047] Figure 1 The image shows the microstructure of sponge spicules; where A, B, C, D, and E are scanning electron microscope images of sponge spicules, with scale bars of 1 μm, 10 μm, 1 μm, 2 μm, and 2 μm, respectively, and F is a micrograph of sponge spicules.

[0048] Figure 2 This is an image of the toothpaste prepared in Example 1.

[0049] Figure 3 This is the result of an antibacterial experiment.

[0050] Figure 4 The gingival condition of rats in each group after toothpaste intervention is shown; where A: normal control group, B: gingivitis model group, and C: experimental group.

[0051] Figure 5 The gingival bleeding index and gingival sulcus depth of rats in each group after toothpaste intervention were measured. Detailed Implementation

[0052] The specific embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0053] The sponge needles used in the examples were a mixture of different lengths and diameters, with an average length of 300 μm and an average diameter of 15 μm. For example... Figure 1 As shown, the sponge spicule exhibits a slender, one-dimensional morphology in its microstructure, appearing as a needle-like or fibrous structure overall. One end of the sponge spicule is open (…). Figure 1 D) The other end is closed and pointed ( Figure 1 E), with a continuous cavity inside ( Figure 1 The shaded area marked by the red box in C indicates that the interior of the sponge needle is a continuous hollow cavity, forming a hollow microneedle structure. This structure can contain, load, and deliver Coptis chinensis extract and other components in toothpaste, enabling quantitative loading and controlled release of active ingredients.

[0054] During use, the tips of the sponge needles come into contact with the oral mucosa. Under the mechanical action of brushing, they can pierce the keratin barrier of the mucosal surface, forming a micron-sized temporary channel. This reduces the physical barrier resistance of the oral mucosa and promotes the penetration and absorption of active ingredients such as Coptis chinensis extract into the oral mucosal tissue. This allows the antibacterial and anti-inflammatory effects of Coptis chinensis to be utilized, achieving targeted delivery to the oral cavity and enhancing the care and efficacy of Coptis chinensis toothpaste.

[0055] In this embodiment, a magnetic stirrer is used for stirring.

[0056] Example 1

[0057] A toothpaste containing microneedles made from the following components in parts by weight: 35 parts sorbitol (humectant), 14 parts hydrated silica, 7 parts thickening silica, 7 parts glycerin (humectant), 2 parts sodium lauryl sulfate, 1.3 parts sodium carboxymethyl cellulose (thickener), 1.6 parts cocamidopropyl betaine, 1 part sponge needles, 0.5 parts lemon flavor, 0.3 parts menthol, 0.2 parts peppermint oil, 0.2 parts xanthan gum (thickener), 0.1 parts sodium benzoate, 0.1 parts sucralose, 0.1 parts coptis extract, and 29.6 parts ultrapure water.

[0058] Preparation method:

[0059] Step 1: Preparation of Coptis chinensis extract: Wash Coptis chinensis with water, dry, pulverize, and pass through a 120-mesh sieve to obtain Coptis chinensis powder; weigh 60 g of Coptis chinensis powder, add 10 times the volume (600 mL) of 70% ethanol by weight of the medicinal material, and reflux extract twice at 80 ℃, each extraction for 1 h. After each extraction, filter, combine the filtrates, concentrate under reduced pressure at 50 ℃, and vacuum dry to obtain Coptis chinensis extract;

[0060] Step 2: Dissolve sucralose, sodium benzoate and Coptis chinensis extract in ultrapure water by stirring at 800 rpm to obtain solution A;

[0061] Step 3: Mix sorbitol and glycerin evenly to obtain a humectant mixture solution; mix sodium carboxymethyl cellulose and xanthan gum evenly; add the evenly mixed thickener to the humectant mixture solution; stir at 75℃ and 800 rpm until evenly mixed to obtain solution B;

[0062] Step 4: Add solution A to solution B while stirring at 1200 rpm. Stir rapidly until the mixture is homogeneous. Homogenize using probe-type ultrasound (ultrasound power 500 W, ultrasound frequency 20 KHz, ultrasound time 3 min (pulse mode 1:2), ice bath maintained at 25℃) until no particles are present, to obtain substance C.

[0063] Step 5: Add hydrated silica, thickening silica, sodium lauryl sulfate, and cocamidopropyl betaine to substance C, and stir at 1200 rpm until completely mixed. Add sponge needles, and stir slowly at 100 rpm until evenly mixed. Finally, add menthol, lemon flavoring, and peppermint oil, and continue stirring at 100 rpm until stringy. Deaerate to obtain Coptis chinensis toothpaste containing microneedles.

[0064] Step Six: The toothpaste paste is filled and sealed to obtain the toothpaste product.

[0065] Example 2

[0066] A Coptis chinensis toothpaste containing microneedles is made from the following components in parts by weight: 35 parts sorbitol, 14.5 parts hydrated silica, 7 parts thickening silica, 7 parts glycerin, 2 parts sodium lauryl sulfate, 1.3 parts sodium carboxymethyl cellulose, 1.6 parts cocamidopropyl betaine, 0.5 parts sponge needles, 0.5 parts lemon flavoring, 0.3 parts menthol, 0.2 parts peppermint oil, 0.2 parts xanthan gum, 0.1 parts sodium benzoate, 0.1 parts sucralose, 0.1 parts Coptis chinensis extract, and 29.6 parts ultrapure water.

[0067] Coptis chinensis toothpaste containing microneedles was prepared according to the method in Example 1.

[0068] Example 3

[0069] A toothpaste containing microneedles made from the following components in parts by weight: 40 parts sorbitol, 13.9 parts hydrated silica, 7 parts thickening silica, 7 parts glycerin, 2 parts sodium lauryl sulfate, 2 parts cocamidopropyl betaine, 1.3 parts sodium carboxymethyl cellulose, 0.5 parts sponge needles, 0.2 parts menthol, 0.2 parts xanthan gum, 0.1 parts lemon flavor, 0.1 parts sodium benzoate, 0.1 parts sucralose, 0.1 parts coptis extract, and 25.5 parts ultrapure water.

[0070] Coptis chinensis toothpaste containing microneedles was prepared according to the method in Example 1.

[0071] Example 4

[0072] A toothpaste containing microneedles made from the following components in parts by weight: 40 parts sorbitol, 13.4 parts hydrated silica, 7 parts thickening silica, 7 parts glycerin, 2 parts sodium lauryl sulfate, 2 parts cocamidopropyl betaine, 1.3 parts sodium carboxymethyl cellulose, 1 part sponge needles, 0.2 parts peppermint oil, 0.2 parts xanthan gum, 0.1 parts lemon flavoring, 0.1 parts sodium benzoate, 0.1 parts sucralose, 0.1 parts coptis extract, and 25.5 parts ultrapure water.

[0073] Coptis chinensis toothpaste containing microneedles was prepared according to the method in Example 1.

[0074] Comparative Example 1

[0075] A Coptis chinensis toothpaste is made from the following components in parts by weight: 35 parts sorbitol, 15 parts hydrated silica, 7 parts thickening silica, 7 parts glycerin, 2 parts sodium lauryl sulfate, 1.3 parts sodium carboxymethyl cellulose, 1.6 parts cocamidopropyl betaine, 0.5 parts lemon flavoring, 0.3 parts menthol, 0.2 parts peppermint oil, 0.2 parts xanthan gum, 0.1 parts sodium benzoate, 0.1 parts sucralose, 0.1 parts Coptis chinensis extract, and 29.6 parts ultrapure water.

[0076] Coptis chinensis toothpaste was prepared according to the method in Example 1.

[0077] Example 5

[0078] 1. Sensory evaluation of toothpaste

[0079] Based on the principles for evaluating toothpaste characteristics in the national standard GB / T 8372-2017 Toothpaste, and considering the characteristics of this product, a detailed scoring rule for sensory evaluation of toothpaste was formulated (Table 1). Twenty testers were randomly selected to conduct sensory evaluations on six toothpaste samples—Examples 1, 2, 3, and 4, and commercially available toothpaste (Control 1: Chenxiang Coptis Toothpaste, Hubei Zhongyanke Pharmaceutical Co., Ltd.; Control 2: Tianqi Herbal Coptis Toothpaste, Zhuji Hongkang Biotechnology Co., Ltd.)—from four aspects: appearance, aroma, taste, and foam volume. The testers' evaluations of the toothpaste were collected, and the results are shown in Table 2.

[0080] The results showed that the toothpastes prepared in Examples 1 and 2 had higher total sensory evaluation scores, and the toothpaste prepared in Example 1 achieved the highest total score in the sensory evaluation. Its overall taste was more in line with popular preferences and had good sensory acceptability.

[0081] Table 1. Sensory Evaluation Scoring Criteria for Toothpaste

[0082]

[0083] Table 2. Taste Rating Results

[0084]

[0085] 2. Antibacterial effect

[0086] (1) Minimum inhibitory concentration (MIC) detection

[0087] Test subjects: toothpaste prepared in Example 1 and Example 2, and toothpaste prepared in Comparative Example 1.

[0088] Test strains: Staphylococcus aureus, Proteus vulgaris, and Candida albicans; Staphylococcus aureus and Proteus vulgaris were cultured on NB medium, while Candida albicans was cultured on SDB medium.

[0089] Sample preparation: Weigh 10 g of toothpaste, mix it with 10 mL of physiological saline, stir thoroughly, and take the supernatant, which is the toothpaste extract (concentration of 1 mg / mL), for later use.

[0090] Bacterial culture: Take the bacterial strain to be tested from the slant with an inoculation loop and inoculate it onto agar medium. Incubate bacteria overnight at 37 ℃ and fungi overnight at 26 ℃.

[0091] Preparation of bacterial suspension: Several morphologically typical single colonies were picked from overnight incubated agar plates and inoculated into an appropriate amount of physiological saline to prepare a bacterial suspension. The turbidity of the bacterial suspension was adjusted to 0.5 McFarland units using a McFarland turbidimeter, and then diluted 1:10000 by volume to a final concentration of approximately 1.5 × 10⁻⁶ units. 4 CFU / mL, for later use.

[0092] To determine the minimum inhibitory concentration (MIC) against different bacteria, the experimental procedure was as follows: Take nine sterile EP tubes and add 1 mL of sterile culture medium to each. Add 1 mL of toothpaste extract to the first tube, mix well, and then transfer 1 mL to the second tube. Dilute sequentially with sterile culture medium in each tube, two-fold, until the seventh tube. The concentrations of the toothpaste extract in each tube at this point are 500.00, 250.00, 125.00, 62.50, 31.25, 15.63, and 7.81 mg / mL, respectively. Figure 3 As shown, 10 µL of bacterial suspension was added to each of tubes 1 to 7; tube 8 was added only with culture medium and bacterial suspension as a drug-free positive control; tube 9 was added with culture medium and toothpaste extract as a sterile negative control.

[0093] The results are shown in Table 3, indicating that the MIC values ​​of the toothpaste containing microneedles in Examples 1 and 2 were significantly lower than those of the toothpaste without microneedles in Comparative Example 1. This suggests that the sponge bone needles can enhance the antibacterial efficacy of Coptis chinensis toothpaste, and the effect is positively correlated with the amount of microneedles added.

[0094] Table 3. Minimum Inhibitory Concentration

[0095]

[0096] (2) Paper method

[0097] Test subjects: toothpaste prepared in Example 1 and commercially available toothpaste (Control 1, Control 2).

[0098] Test strains: Staphylococcus aureus, Proteus vulgaris, and Candida albicans.

[0099] Preparation of bacterial suspension: Prepare bacterial suspension (1.5 × 10⁻⁶) according to "(1) Minimum inhibitory concentration detection". 8 (CFU / mL).

[0100] Sample preparation: Weigh 1 g of toothpaste, add physiological saline to 10 mL to a concentration of 10% (w / v), stir thoroughly, and take the supernatant, which is the toothpaste stock solution, for later use; take a 7 mm diameter sterile dry filter paper, add 20 μL of toothpaste stock solution to each paper as the test sample (i.e., drug paper), and add an equal volume of sterile physiological saline to the blank control.

[0101] Plate inoculation: Use a pipette to draw 100 μL of bacterial suspension (1.5 × 10⁻⁶).8 (CFU / mL) of the drug was spread evenly three times on the surface of the corresponding nutrient agar plates. The plates were then covered and left to stand for about 5 minutes to allow the agar surface to dry. According to the groups, drug-coated paper discs were placed on the surface of the inoculated agar, ensuring complete contact between each disc and the agar surface. Each group was repeated three times. After placing the discs, the plates were covered, sealed with sealing film, and incubated in a constant temperature incubator for 16-18 hours. The diameter of the inhibition zone was observed and measured, and the average value was recorded. The larger the diameter of the inhibition zone, the stronger the antibacterial ability.

[0102] The results are shown in Table 4. It can be seen that, compared with commercially available toothpaste, the toothpaste of Example 1 has the largest diameter of inhibition rings against Staphylococcus aureus, Proteus vulgaris, and Candida albicans, indicating that the toothpaste of Example 1 has the best antibacterial effect and that its antibacterial performance is superior to that of commercially available toothpaste.

[0103] Table 4. Results of the antibacterial test (inhibition zone diameter: mm)

[0104]

[0105] 3. Anti-gingivitis effect

[0106] (1) Experimental animals: 7-8 week old male SD rats.

[0107] (2) Experimental Procedure: SD rats were first acclimatized for one week, and then 21 SD rats were randomly divided into a normal control group, a gingivitis model group, and a toothpaste group, with 7 rats in each group. The normal control group rats were not treated. In both the gingivitis model group and the toothpaste group, the maxillary second molars were ligated using orthodontic wire ligation to establish a rat gingivitis model, with the contralateral corresponding tooth as a control. The gingival status (including color, texture, and morphology) of the bilateral maxillary second molars of the rats was observed visually, and the gingival bleeding index and gingival sulcus depth were measured and recorded. Two weeks later, the gingival color, texture, and morphology of the bilateral maxillary second molars of the rats were observed, and the gingival bleeding index and gingival sulcus depth were measured and recorded to verify the successful establishment of the rat gingivitis model.

[0108] After successful modeling, drug administration was performed: Rats in the normal control group and periodontitis model group received no drug treatment. Toothpaste group: 0.1 g of the toothpaste prepared in Example 1 was applied evenly to the affected area of ​​the gingivitis in rats twice daily for 7 days. 24 hours after administration on day 7, the gingival color, texture, and morphology of the bilateral maxillary second molars were observed again visually, and the gingival bleeding index and gingival sulcus depth were measured and recorded.

[0109] Gingival bleeding index was measured using a dental double-ended probe and scored according to the following criteria (average calculated by summing the values ​​at each point): 0: normal gingiva; 1: gingival edema, but no bleeding after probing; 2: bleeding after probing; 3: spontaneous gingival bleeding or ulceration. Gingival sulcus depth: The maxillary second molar of rats was probed. The periodontal pocket depth was measured using a periodontal probe at six sites: mesial, central, and distal on the buccal side and mesial, central, and distal on the palatal side. The periodontal pocket depth is the distance from the gingival margin to the bottom of the pocket. The measurements were recorded and the average depth was taken.

[0110] All experimental data were analyzed using SPSS Statistics 27.0 software. One-way ANOVA was used to compare different groups, and p < 0.05 was considered statistically significant.

[0111] (3) Experimental Results

[0112] One week after administration, visual observation revealed no significant changes in the gingiva of rats in the normal control group, while the gingiva of rats in the periodontitis model group was red and swollen, with bleeding upon touch. In contrast, the gingiva of rats in the toothpaste group became lighter in color, harder in texture, and the degree of edema was reduced. Figure 4 After drug administration, there were significant differences in gingival bleeding index (GI) and gingival sulcus depth (PD) among the groups (p<0.05) (Table 5). Figure 5 ).

[0113] Table 5. Comparison of gingival bleeding index and gingival sulcus depth among rats in each group after drug treatment ( (n=7)

[0114] .

Claims

1. A toothpaste containing microneedles made from Coptis chinensis, characterized in that: It is made from the following components in parts by weight: 40-50 parts humectant, 20-30 parts abrasive, 1-2 parts thickener, 3-4 parts foaming agent, 0.1-0.3 parts sweetener, 0.1-1 parts Coptis chinensis extract, 0.1-1 parts sponge spicules, 0.2-0.6 parts menthol, 0.2-0.6 parts peppermint oil, 0.1-0.6 parts fruit flavoring, 0.1-0.2 parts preservative, and 20-30 parts ultrapure water; wherein the Coptis chinensis extract is a 70% ethanol extract of Coptis chinensis; the humectant is at least one of sorbitol and glycerin; the abrasive is at least one of hydrated silica, silica, and calcium hydrogen phosphate; and the foaming agent is at least one of sodium lauryl sulfate, sodium lauroyl sarcosinate, and cocamidopropyl betaine.

2. The Coptis chinensis toothpaste containing microneedles according to claim 1, characterized in that: It is made from the following components in parts by weight: 40-45 parts humectant, 21-22 parts abrasive, 1-2 parts thickener, 3-3.6 parts foaming agent, 0.1-0.3 parts sweetener, 0.1-1 parts Coptis chinensis extract, 0.1-1 parts sponge spicules, 0.2-0.6 parts menthol, 0.2-0.6 parts peppermint oil, 0.1-0.6 parts fruit flavoring, 0.1-0.2 parts preservative, and 20-30 parts ultrapure water.

3. The Coptis chinensis toothpaste containing microneedles according to claim 1 or 2, characterized in that: The Coptis chinensis extract is obtained by crushing Coptis chinensis, passing it through a 120-mesh sieve, refluxing it twice with 70% ethanol as the extraction solvent for 1 hour each time, filtering it, concentrating the filtrate under reduced pressure, and drying it under vacuum.

4. The Coptis chinensis toothpaste containing microneedles according to claim 1 or 2, characterized in that: The sponge bone needles are porous silica bone needles with an average length of 200-300 μm and an average diameter of 15-20 μm.

5. The Coptis chinensis toothpaste containing microneedles according to claim 1 or 2, characterized in that: The moisturizer is a combination of sorbitol and glycerin in a weight ratio of 5:1 to 6:1, preferably a combination of sorbitol and glycerin in a weight ratio of 5:

1.

6. The Coptis chinensis toothpaste containing microneedles according to claim 1 or 2, characterized in that: The friction agent is a combination of hydrated silica and silicon dioxide in a weight ratio of 1.8:1 to 2.2:1, preferably a combination of hydrated silica and silicon dioxide in a weight ratio of 2:1 to 2.2:

1.

7. The Coptis chinensis toothpaste containing microneedles according to claim 1 or 2, characterized in that: The foaming agent is a combination of sodium lauryl sulfate and cocamidopropyl betaine in a weight ratio of 1:0.8 to 1:1, preferably a combination of sodium lauryl sulfate and cocamidopropyl betaine in a weight ratio of 1:0.

8.

8. The Coptis chinensis toothpaste containing microneedles according to claim 1 or 2, characterized in that: The thickener is at least one of sodium carboxymethyl cellulose, carrageenan, and xanthan gum; the sweetener is sucralose; the fruit flavoring is at least one of lemon flavoring and peach flavoring; and the preservative is sodium benzoate.

9. A toothpaste containing microneedles made from Coptis chinensis, characterized in that: It is made from the following components in parts by weight: 35 parts sorbitol, 7 parts glycerin, 14 parts hydrated silica, 7 parts thickening silica, 1.3 parts sodium carboxymethyl cellulose, 0.2 parts xanthan gum, 2 parts sodium lauryl sulfate, 1.6 parts cocamidopropyl betaine, 1 part sponge spicule, 0.3 parts menthol, 0.2 parts peppermint oil, 0.5 parts lemon flavor, 0.1 parts sodium benzoate, 0.1 parts sucralose, 0.1 parts Coptis chinensis extract, and 29.6 parts ultrapure water; wherein the Coptis chinensis extract is a 70% ethanol extract of Coptis chinensis.

10. A method for preparing Coptis chinensis toothpaste containing microneedles as described in claim 1, characterized in that: Includes the following steps: Step 1: Dissolve the sweetener, preservative, and Coptis chinensis extract in ultrapure water to obtain solution A; Step 2: Add the thickener to the humectant and stir at 70-80℃ until the mixture is homogeneous to obtain solution B; Step 3: While stirring, add solution A to solution B, stir quickly until the mixture is uniform, and then homogenize until there are no particles to obtain substance C; Step 4: Add the abrasive and foaming agent to substance C and stir until evenly mixed. Add the sponge needles and stir evenly. Finally, add menthol, fruit flavoring, and peppermint oil, and continue stirring until stringy. Deaerate to obtain Coptis chinensis toothpaste containing microneedles. Step 5: Filling and sealing to obtain the finished toothpaste.

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