Compound honeysuckle flower toothpaste for treating oral ulcer and dental caries and preparation method thereof

Abstract

This invention belongs to the field of toothpaste technology, specifically relating to a compound honeysuckle herbal toothpaste for treating oral ulcers and dental caries, and its preparation method. The toothpaste contains the following ingredients: honeysuckle extract, angelica dahurica extract, bletilla striata extract, licorice extract, cellulose gum, sorbitol, sodium monofluorophosphate, sodium benzoate, hydrated silica, sodium lauryl sulfate, sodium saccharin, and deionized water. The preparation process includes ultrafine grinding, two water extractions, low-temperature concentration, and graded filtration to prepare the herbal extracts, which are then mixed and homogenized with a matrix to obtain a stable gel paste. This process improves the extraction of beneficial components from the herbal extracts and achieves synergistic effects on multiple targets. This novel formulation has been demonstrated in rat oral ulcer experiments to significantly reduce ulcer diameter, accelerate healing, and reduce irritation. It has a mild and safe effect on the oral mucosa and is suitable for daily care in people prone to oral ulcers and those with sensitive mouths. This invention has a scientifically formulated, stable, and effective formula with promising application prospects.

Description

Technical Field

[0001] This invention relates to the field of toothpaste, specifically to a compound honeysuckle herbal toothpaste for treating oral ulcers and dental caries, and its preparation method. Background Technology

[0002] Oral ulcers, a common and frequently occurring oral mucosal lesion, are characterized by recurrent attacks, significant pain, and long healing periods, significantly impacting patients' daily eating, communication, and quality of life. Currently, most oral care products for oral ulcers rely on chemical antibacterial and analgesic ingredients. While they can provide short-term symptom relief, they generally suffer from strong irritation, easily damage the ulcer mucosa, and disrupt the normal oral flora with long-term use. Furthermore, their single-target action limits their ability to promote ulcer mucosal repair, making it difficult to achieve a comprehensive and effective treatment.

[0003] While existing oral care products based on traditional Chinese medicine have improved in terms of gentleness, they still have significant shortcomings: most formulas are not precisely formulated for oral ulcers, resulting in weak synergy among anti-inflammatory, analgesic, and repairing effects, and poor healing promotion; some products have simple extraction processes for traditional Chinese medicine, low utilization rate of effective ingredients, and poor stability and oral biocompatibility of the paste; and some products only focus on gingival inflammation and gingival bleeding, lacking specific designs for the protection of oral ulcer wounds and mucosal regeneration, thus failing to meet the actual care needs of high-incidence populations of ulcers.

[0004] The scientific combination of four medicinal herbs—honeysuckle, bletilla, angelica, and licorice—can achieve synergistic effects on multiple targets, specifically addressing the core issues of oral ulcers such as inflammation, pain, and slow healing.

[0005] Dental caries, commonly known as cavities or tooth decay, is a progressive lesion of the hard tissues of the teeth caused by a combination of factors in the oral cavity. It is a major and common oral disease in humans and one of the most prevalent diseases. Currently, fluoride toothpaste or fluoride products are commonly used to address this problem, and these products can reduce the incidence of dental caries by about 40%. Fluorides include sodium fluoride, potassium fluoride, stannous fluoride, and sodium monofluorophosphate. This invention uses sodium monofluorophosphate as the fluoride.

[0006] Therefore, this invention provides a toothpaste with honeysuckle compound as its core, which effectively overcomes the shortcomings of existing products such as high irritation, single efficacy, weak healing effect, and insufficient targeted compatibility. It also has the advantages of being mild and safe, effective, and stable, and has outstanding creative and practical value. Summary of the Invention

[0007] To address the problems of existing toothpastes being highly irritating and having poor ulcer healing effects, this invention provides a compound honeysuckle toothpaste formula and its preparation method. Through the synergistic effect of natural Chinese herbal ingredients, it achieves mild antibacterial effects, promotes ulcer healing, and relieves pain, while also being highly safe.

[0008] In view of this, one of the objectives of the present invention is to provide a compound honeysuckle toothpaste, which is composed of extracts of traditional Chinese medicine and a toothpaste base;

[0009] The Chinese herbal extract is prepared by the following steps: by weight, prepare 1.5 parts of honeysuckle, 1 part of angelica, 1 part of bletilla, and 0.5 parts of licorice, for a total of 4 parts. Mix the herbs and pulverize them into ultrafine powder. After soaking and pretreatment, two water extractions, graded filtration, and low-temperature concentration, the Chinese herbal extract is obtained.

[0010] The ultrafine pulverization process involves pulverizing the four mixed portions of Chinese medicinal materials using a Chinese medicine pulverizer (120 mesh), pulverizing each batch for 30 seconds, stopping for 10 seconds, repeating this process three times, and then sieving the mixture.

[0011] The soaking pretreatment is as follows: add 40 parts of deionized water, let stand and soak at 25±2℃ for 2 hours, and stir with a magnetic stirrer for 1 minute each at 30 min, 60 min and 90 min to ensure that the particles completely sink and retain the soaking water;

[0012] The process of the two water extractions is as follows: the extraction is carried out in two stages. For the first stage, deionized water is added to 48 parts, the temperature is kept constant at 60±2℃ for 1 hour, then gently boiled at 95-100℃ for 1.5 hours, and then filtered to obtain the filtrate. For the second stage, 32 parts of deionized water are added, the extraction parameters are repeated, and the filtrates are combined to obtain ≥40 parts.

[0013] The graded filtration process is as follows: first, coarse filtration through 4 layers of sterile gauze, then filtration through a 0.22μm filter membrane until clear; if the viscosity is ≥500mPa.s, 0.1% activated carbon by weight of the filtrate is added for purification.

[0014] Low-temperature concentration: Concentrate at 45±2℃ and a vacuum of 0.09MPa to a relative density of 1.1-1.2 (60℃, atmospheric pressure).

[0015] The toothpaste matrix is ​​prepared by the following steps: 2.75 parts of cellulose gum are dissolved in 25 parts of deionized water at 45-50℃ and stirred until there are no particles and no layering, forming a colloid (viscosity 8000-10000 mPa.s) to obtain a cellulose gum solution for later use; 25 parts of sorbitol are dissolved in 3 parts of deionized water, and then 16.5 parts of hydrated silica, 1.25 parts of sodium lauryl sulfate, 4 parts of sodium saccharin, sodium benzoate solution (pre-dissolved in 3 parts of deionized water at 50℃ to obtain 0.4 parts of sodium benzoate), and 0.7 parts of sodium monofluorophosphate are added sequentially. The mixture is stirred for 1 minute until completely dissolved, then the prepared cellulose gum solution is added, followed by 39-41 parts of deionized water. The mixture is then stirred at 25℃ for 15 minutes to obtain a matrix suspension with a viscosity of 3000-4000 mPa.s.

[0016] Preferably, the raw materials for preparing the toothpaste matrix meet the following requirements: cellulose gum viscosity ≥ 5000 mPa.s, sorbitol purity ≥ 98%, hydrated silica particle size 5-15 μm, Mohs hardness ≤ 3, sodium lauryl sulfate purity ≥ 95%, sodium saccharin and sodium benzoate purity ≥ 99%, sodium monofluorophosphate is toothpaste industrial grade, conforms to GB24567-2009 requirements, purity ≥ 98.0%, total fluoride in the finished product is controlled at 0.05%-0.15%, deionized water conductivity ≤ 10 μS / cm, pH 6.5-7.5.

[0017] The second objective of this invention is to provide a method for preparing the compound honeysuckle toothpaste described above, comprising the following steps:

[0018] S1. Preparation of Chinese herbal extracts: By weight, 1.5 parts of honeysuckle, 1 part of angelica dahurica, 1 part of bletilla striata, and 0.5 parts of licorice, totaling 4 parts, are mixed and ultra-finely pulverized. After soaking, two water extractions, graded filtration, and low-temperature concentration, 5-5.85 parts of Chinese herbal concentrate are obtained.

[0019] The ultrafine pulverization process involves mixing four portions of Chinese medicinal herbs, pulverizing them using a Chinese medicine pulverizer (120 mesh), pulverizing each batch for 30 seconds, stopping for 10 seconds, repeating this process three times, and then sieving.

[0020] The soaking pretreatment is as follows: add 40 parts of deionized water, let stand and soak at 25±2℃ for 2 hours, and stir with a magnetic stirrer for 1 minute each at 30 min, 60 min and 90 min to ensure that the particles completely sink.

[0021] The process of the two water extractions is as follows: the extraction is carried out in two stages. For the first stage, deionized water is added to 48 parts, the temperature is kept constant at 60±2℃ for 1 hour, then gently boiled at 95-100℃ for 1.5 hours, and then filtered to obtain the filtrate. For the second stage, 32 parts of deionized water are added, the extraction parameters are repeated, and the filtrates are combined to obtain ≥40 parts.

[0022] The graded filtration process is as follows: first, coarse filtration through 4 layers of sterile gauze, then filtration through a 0.22μm filter membrane until clear; if the viscosity is ≥500mPa.s, 0.1% activated carbon by weight of the filtrate is added for purification.

[0023] The low-temperature concentration is carried out at 45±2℃ and a vacuum of 0.09MPa until the relative density is 1.1-1.2 (60℃).

[0024] S2. Toothpaste matrix preparation: Dissolve 2.75 parts of cellulose gum in 25 parts of deionized water at 45-50℃ and stir until there are no particles and no layering, forming a colloid (viscosity 8000-10000 mPa.s) to obtain a cellulose gum solution for later use; dissolve 25 parts of sorbitol in 3 parts of deionized water, then add 16.5 parts of hydrated silica, 1.25 parts of sodium lauryl sulfate, 4 parts of sodium saccharin, sodium benzoate solution (pre-dissolve 0.4 parts of sodium benzoate in 3 parts of deionized water at 50℃ to obtain a sodium benzoate solution), and 0.7 parts of sodium monofluorophosphate in sequence, stir for 1 minute until completely dissolved, then add the prepared cellulose gum solution, then add 39-41 parts of deionized water, and stir at 25℃ for 15 minutes to obtain a matrix suspension with a viscosity of 3000-4000 mPa.s;

[0025] S3. Mixing and homogenization: The Chinese herbal concentrate at 45℃ was added to the matrix suspension in three portions and stirred at 200r / min for 15min. The viscosity was measured to be 5000-8000mPa.s. The mixture was then transferred to a homogenizer and homogenized at 12000r / min for 10min. The cup wall was scraped at the 3rd and 6th minutes to ensure that there were no particles ≥50μm and no stratification, thus obtaining the compound honeysuckle toothpaste.

[0026] Furthermore, the toothpaste matrix described in step S2 meets the following requirements: cellulose gum viscosity ≥ 5000 mPa.s, sorbitol purity ≥ 98%, hydrated silica particle size 5–15 μm, Mohs hardness ≤ 3, sodium lauryl sulfate purity ≥ 95%, sodium saccharin and sodium benzoate purity ≥ 99%, sodium monofluorophosphate is toothpaste industrial grade, conforms to GB24567-2009 requirements, purity ≥ 98.0%, total fluoride in the finished product is controlled at 0.05%–0.15%, deionized water conductivity ≤ 10 μS / cm, pH 6.5–7.5.

[0027] The third objective of this invention is to provide the application of the above-mentioned compound honeysuckle toothpaste in oral care, or in the preparation of oral care products, or in the preparation of products or drugs for the prevention and treatment of ulcers and dental caries.

[0028] The fourth objective of this invention is to provide a Chinese herbal extract, which is prepared by the following method: by weight, prepare 1.5 parts of honeysuckle, 1 part of angelica dahurica, 1 part of bletilla striata, and 0.5 parts of licorice, totaling 4 parts; mix the herbs and pulverize them into ultrafine powder; after soaking pretreatment, two water extractions, graded filtration, and low-temperature concentration, a Chinese herbal extract is obtained.

[0029] The ultrafine pulverization process involves pulverizing the four mixed portions of Chinese medicinal materials using a Chinese medicine pulverizer (120 mesh), pulverizing each batch for 30 seconds, stopping for 10 seconds, repeating this process three times, and then sieving the mixture.

[0030] The soaking pretreatment is as follows: add 40 parts of deionized water, let stand and soak at 25±2℃ for 2 hours, and stir with a magnetic stirrer for 1 minute each at 30 min, 60 min and 90 min to ensure that the particles completely sink and retain the soaking water;

[0031] The process of the two water extractions is as follows: the extraction is carried out in two stages. For the first stage, deionized water is added to 48 parts, the temperature is kept constant at 60±2℃ for 1 hour, then gently boiled at 95-100℃ for 1.5 hours, and then filtered to obtain the filtrate. For the second stage, 32 parts of deionized water are added, the extraction parameters are repeated, and the filtrates are combined to obtain ≥40 parts.

[0032] The graded filtration process is as follows: first, coarse filtration through 4 layers of sterile gauze, then filtration through a 0.22μm filter membrane until clear; if the viscosity is ≥500mPa.s, 0.1% activated carbon by weight of the filtrate is added for purification.

[0033] The low-temperature concentration is carried out at 45±2℃ and a vacuum of 0.09MPa until the relative density is 1.1-1.2 (60℃, normal pressure).

[0034] The fifth objective of this invention is to provide the application of the above-mentioned Chinese herbal extracts in oral care, or in the preparation of oral care products, or in the preparation of products or drugs for the prevention and treatment of ulcers and dental caries.

[0035] Beneficial effects

[0036] This invention provides a compound honeysuckle toothpaste, which scientifically combines four medicinal herbs—honeysuckle, angelica, bletilla, and licorice—to work synergistically with the toothpaste base to achieve multiple effects such as relieving oral ulcers, reducing inflammation, and preventing tooth decay. It solves the technical problems of oral ulcers being prone to recurrence, causing significant pain, slow healing, and the strong irritation of conventional oral care products.

[0037] This invention uses honeysuckle as the core anti-inflammatory component, while the other three Chinese herbs work synergistically to exert their effects.

[0038] The toothpaste base of this invention adopts a mild and safe system: cellulose gum is used as a gelling agent to ensure stable viscosity and good formability of the paste; sorbitol is used as a humectant to prevent the paste from drying out and to improve the smoothness of use; hydrated silica is used as a low-hardness abrasive with moderate particle size and mild hardness, cleaning tooth stains without damaging tooth enamel and ulcers; an appropriate amount of surfactant is added to enhance foaming ability, sweeteners to enrich the taste, and preservatives to extend shelf life; sodium monofluorophosphate is added to provide fluoride for anti-caries effect. The formula contains no strong irritating ingredients, and the pH is close to the physiological environment in the oral cavity, making it suitable for various fragile conditions such as oral ulcers and oral sensitivity.

[0039] Verified by rat oral ulcer experiments, the compound honeysuckle toothpaste formula of this invention has anti-ulcer and anti-inflammatory effects, which can significantly reduce the diameter of ulcers, reduce the degree of inflammation, and effectively shorten the ulcer healing cycle. Long-term use does not cause mucosal irritation or allergic reactions, does not disrupt the normal oral microecology, and is safe and harmless to oral tissues. It combines nursing and safety, and is suitable for daily long-term use by people prone to oral ulcers and people with sensitive mouths. Attached Figure Description

[0040] Figure 1 The mice in this invention's model group;

[0041] Figure 2 Mice used in the toothpaste group of this invention;

[0042] Figure 3 This represents the change in ulcer area over time among the mice in each group of the present invention. Detailed Implementation

[0043] The present invention will be described in detail below with reference to embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of application of the present invention. The present invention is not limited to the following embodiments or examples. Any modifications and variations made without departing from the spirit of the present invention should be included within the scope of the present invention. Unless otherwise specified, the experimental materials or reagents used in the following embodiments are all conventional commercially available products. All "parts" in the following embodiments are by weight, i.e., "parts" refers to parts by weight.

[0044] Information and sources of the main materials or reagents used in this embodiment:

[0045] Honeysuckle: Category: Traditional Chinese Medicine Slices, Xiushan County, Chongqing;

[0046] Angelica dahurica: Category: Traditional Chinese medicine decoction pieces, Sichuan Zhuoyu Pharmaceutical Co., Ltd., batch number: 240903;

[0047] Bletilla striata: Category: Traditional Chinese medicine decoction pieces, Sichuan Pufengtang Pharmaceutical Co., Ltd., batch number: 220501;

[0048] Licorice: Category: Traditional Chinese Medicine Slices, Sichuan Zhuoyu Pharmaceutical Co., Ltd., Batch No.: 250304;

[0049] Hydrated silica: Guangzhou Haohuang Co., Ltd., 103 type semi-transparent, state: powder;

[0050] Cellulose gum, sodium benzoate, sodium saccharin, sodium lauryl sulfate, sorbitol: Maclean, state: powder.

[0051] Example 1 (Baseline Formulation)

[0052] The preparation method of the compound honeysuckle toothpaste in this embodiment is carried out according to the following steps:

[0053] S1. Preparation of Chinese herbal extract: 1.5 parts of honeysuckle, 1 part of angelica dahurica, 1 part of bletilla striata, and 0.5 parts of licorice, totaling 4 parts. The herbs were mixed and ultra-finely pulverized, then pretreated by soaking, extracted twice with water, filtered in stages, and concentrated at low temperature to obtain a concentrated Chinese herbal extract. The specific operation is as follows:

[0054] Ultrafine grinding: Grind the four mixed Chinese medicinal materials with a Chinese medicine pulverizer (120 mesh), grinding each batch for 30 seconds and stopping for 10 seconds, repeating 3 times, and then sieving.

[0055] Soaking pretreatment: Add 40 parts of deionized water, let stand and soak for 2 hours at 25±2℃, and stir with a magnetic stirrer for 1 minute each at 30 min, 60 min and 90 min to ensure that the particles completely sink, and retain the soaking water (i.e., do not filter to remove the water).

[0056] Water extraction process: Extraction is performed in two stages. For the first stage, deionized water is added to 48 parts, and the mixture is kept at 60±2℃ for 1 hour, then boiled gently at 95-100℃ for 1.5 hours, and then filtered to obtain the filtrate. For the second stage, 32 parts of deionized water are added, and the extraction parameters are repeated. The filtrates are combined, and the filtrate is ≥40 parts.

[0057] Graded filtration: First, coarsely filter through 4 layers of sterile gauze, then filter through a 0.22μm filter membrane until clear. If the viscosity is ≥500mPa.s, add 0.1% activated carbon by weight of the filtrate for purification.

[0058] Low-temperature concentration: Concentrate at 45±2℃ and vacuum degree 0.09MPa until the relative density is 1.1-1.2 (60℃, normal pressure), resulting in a free-flowing viscous paste that is neither too thin nor too dry and hard. The concentrate mass is approximately 5-5.85 parts. Store at 4℃ for ≤24h.

[0059] S2. Toothpaste matrix preparation: Dissolve 2.75 parts of cellulose gum in 25 parts of deionized water at 45-50℃ and stir until there are no particles and no layering, forming a colloid (viscosity 8000-10000 mPa.s) to obtain a cellulose gum solution for later use; dissolve 25 parts of sorbitol in 3 parts of deionized water, then add 16.5 parts of hydrated silica, 1.25 parts of sodium lauryl sulfate, 4 parts of sodium saccharin, sodium benzoate solution (pre-dissolve 0.4 parts of sodium benzoate in 3 parts of deionized water at 50℃ to obtain a sodium benzoate solution), and 0.7 parts of sodium monofluorophosphate in sequence, stir for 1 minute until completely dissolved, then add the prepared cellulose gum solution, then add 39-41 parts of deionized water, and stir at 25℃ for 15 minutes to obtain a matrix suspension with a viscosity of 3000-4000 mPa.s;

[0060] The raw materials used to prepare the toothpaste base meet the following requirements: cellulose gum viscosity ≥ 5000 mPa.s, sorbitol purity ≥ 98%, hydrated silica particle size 5-15 μm, Mohs hardness ≤ 3, sodium lauryl sulfate purity ≥ 95%, sodium saccharin and sodium benzoate purity ≥ 99%, sodium monofluorophosphate is toothpaste industrial grade, conforms to GB24567-2009 requirements, purity ≥ 98.0%, total fluoride in the finished product is controlled at 0.05%-0.15%, and deionized water conductivity ≤ 10 μS / cm, pH 6.5-7.5.

[0061] S3. Mixing and homogenization: The Chinese herbal medicine concentrate was added to the matrix suspension in three portions at 45℃, and stirred at 200r / min for 15min. The viscosity was measured to be 5000-8000mPa.s.

[0062] Homogenization: Transfer to a homogenizer and homogenize at 12000r / min for 10min. Scrape the cup wall at 3min and 6min to ensure no particles ≥50μm and no stratification, to obtain compound honeysuckle toothpaste.

[0063] Example 2 (High-Hydration Silica Formulation)

[0064] This embodiment provides a compound honeysuckle toothpaste, by total mass. The difference between this embodiment and Embodiment 1 is that the amount of hydrated silica is increased to enhance the cleaning and whitening effects, while the amount of sorbitol is correspondingly reduced to maintain the overall balance of the system. The amounts of other Chinese herbal extracts and excipients are the same as in Embodiment 1.

[0065] The toothpaste base in this embodiment consists of the following components: 2.75 parts cellulose gum, 18.5 parts sorbitol, 23 parts hydrated silica, 1.25 parts sodium lauryl sulfate, 0.7 parts sodium monofluorophosphate, 4 parts sodium saccharin, and 0.4 parts sodium benzoate. The raw materials and dosages used for the herbal extract are exactly the same as in Example 1, namely, 1.5 parts honeysuckle, 1 part angelica dahurica, 1 part bletilla striata, and 0.5 parts licorice.

[0066] The preparation method is the same as in Example 1, except that the stirring time needs to be extended when adding hydrated silica to ensure full dispersion.

[0067] Experimental results show that although the cleaning and whitening effects of the toothpaste obtained in this embodiment are improved, the consistency of the paste is reduced, and slight stratification occurs after long-term storage. It is not suitable for people with a high incidence of oral ulcers.

[0068] Experimental Example 3 (Sodium High Lauryl Sulfate Formulation)

[0069] This embodiment provides a compound honeysuckle toothpaste, by total mass. The difference between this embodiment and Example 1 is that the amount of sodium lauryl sulfate is increased to enhance foaming properties, while the amount of sorbitol is slightly adjusted to maintain the overall balance of the system. The amounts of other Chinese herbal extracts and excipients are the same as in Example 1.

[0070] The toothpaste base in this embodiment consists of the following components: 2.75 parts cellulose gum, 24.2 parts sorbitol, 16.5 parts hydrated silica, 2.0 parts sodium lauryl sulfate, 0.7 parts sodium monofluorophosphate, 4 parts sodium saccharin, and 0.4 parts sodium benzoate. The raw materials and dosages used for the herbal extract are exactly the same as in Example 1, namely 1.5 parts honeysuckle, 1 part angelica dahurica, 1 part bletilla striata, and 0.5 parts licorice.

[0071] The preparation method is the same as in Example 1, except that sodium lauryl sulfate should be added slowly in 4-5 portions while controlling the stirring speed to prevent excessive foam from overflowing.

[0072] Experimental results show that the toothpaste produced in this embodiment produces too much foam, and excessive foam affects brushing comfort, indicating that simply increasing the amount of foaming agent cannot improve the user experience.

[0073] Reasons for choosing Example 1

[0074] A comprehensive comparison reveals that while Comparative Example 1 showed improved cleaning power, it also increased irritation to ulcers and decreased stability; Comparative Example 2 resulted in excessive foaming, leading to a reduced user experience. Example 1 demonstrated a balanced performance across all aspects, ensuring gentle cleaning, appropriate foaming, good stability, and effective ulcer care. Therefore, Example 1 was selected as the optimal formulation.

[0075] Efficacy verification

[0076] 1. Experimental Materials: 32 SD-grade white rats, weighing 200-220g, all female; toothpaste prepared in Example 1 of this invention; the toothpaste prepared in Example 1 of this invention contains only a base (as a blank base for toothpaste) and no traditional Chinese medicine ingredients; 90% phenol solution (ulcer model construction reagent, analytical grade); Beijing Tongrentang Oral Ulcer Powder (positive control drug, National Drug Approval Number Z11020184); 10% chloral hydrate (chemically pure, dosage calculated at 300mg / kg rat body weight, intraperitoneal injection for anesthesia); 0.9% sodium chloride solution (physiological saline); electronic digital caliper (accuracy 0.01mm); electronic balance (range 0-500g, accuracy 0.01g); pipette tip (made into a container with a diameter of approximately 5mm); sterile cotton swabs.

[0077] 2. Ulcer Model Construction: A container approximately 5 mm in diameter was made using a pipette tip, filled with a cotton ball, and soaked in 90% phenol solution until the cotton ball was completely saturated. Rats were anesthetized by intraperitoneal injection of 10% chloral hydrate at a dose of 300 mg / kg. After the corneal reflex disappeared and the limbs relaxed, the rats were fixed in place. The pipette tip containing the phenol-soaked cotton ball was placed vertically in contact with the rat's lower lip mucosa (approximately 4.5 mm × 4.5 mm) for 10 seconds, then removed. Immediately afterward, the cauterized area was gently wiped with a sterile cotton swab dipped in physiological saline to remove residual phenol. After 24 hours, the rats were observed. If ulcers (5.0-5.5 mm in diameter) appeared on the mucosa, covered with a grayish-white pseudomembrane, and surrounded by congestion and edema, the model was considered successfully constructed.

[0078] 3. Experimental Grouping: Thirty-two rats were randomly divided into four groups of eight each: a model control group, a blank toothpaste matrix group, a toothpaste group, and a positive control group. The model control group underwent only ulcer model construction without any intervention; the blank toothpaste matrix group was treated with the toothpaste matrix prepared in Example 1 of this invention, which contained no traditional Chinese medicine ingredients; the toothpaste group was treated with the toothpaste prepared in Example 1 of this invention; and the positive control group was treated with Beijing Tongrentang Oral Ulcer Powder. The dosage for each group was 0.1 g / rat / day.

[0079] 4. Drug Administration and Observation: Drug administration began 24 hours after successful model establishment, twice daily (8-hour intervals). Using sterile cotton swabs, 0.1 g of toothpaste blank matrix, toothpaste, and positive control drug were applied evenly to the ulcers of the corresponding groups of rats. The model control group received no treatment. Rats were fasted for 30 minutes after each administration. The administration was continued for 7 days, and the ulcer diameter was measured daily using calipers (0.01 mm accuracy), and the ulcer healing progress was recorded.

[0080] 5. Data Processing: Experimental data are expressed as mean ± standard deviation. The results indicate that one-way ANOVA was used for statistical testing, and LSD test was used for multiple comparisons between groups. P < 0.05 was considered statistically significant, and P < 0.01 was considered highly statistically significant.

[0081] 6. Experimental Results: The experimental results showed that, compared with the model control group and the blank toothpaste matrix group, the toothpaste prepared in Example 1 of this invention had a significant inhibitory effect on phenol-induced oral ulcers in rats, significantly accelerated ulcer healing speed, and significantly shortened healing time, with statistically significant differences (P < 0.05). The positive control group also showed a significant anti-ulcer effect. Compared with the model control group, there was no significant difference in ulcer healing between the blank toothpaste matrix group and the model control group (P > 0.05), indicating that the healing-promoting effect of the toothpaste matrix was negligible, and the anti-ulcer efficacy mainly came from the synergistic effect of the four traditional Chinese medicines: honeysuckle, angelica, bletilla, and licorice.

[0082] like Figure 3As shown in the figure, statistical analysis revealed significant differences in ulcer area over time among the groups. The toothpaste group showed statistical significance compared to the model group and the matrix group (P<0.05), indicating that the toothpaste described in this invention can significantly promote ulcer healing and has a significantly better therapeutic effect than the blank model and matrix control, with clear statistical significance.

[0083] The conventional techniques and solutions not described in detail in the above embodiments are all well known in the art, and therefore will not be elaborated upon here. The above embodiments and / or experimental examples describe the preferred embodiments of the present invention in detail. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, and these simple modifications all fall within the protection scope of the present invention.

Claims

1. A compound honeysuckle toothpaste, characterized in that, Composed of extracts from traditional Chinese medicinal herbs and toothpaste base; The Chinese herbal extract is prepared by the following steps: by weight, prepare 1.5 parts of honeysuckle, 1 part of angelica, 1 part of bletilla, and 0.5 parts of licorice, for a total of 4 parts. Mix the herbs and pulverize them into ultrafine powder. After soaking and pretreatment, two water extractions, graded filtration, and low-temperature concentration, the Chinese herbal extract is obtained. The ultrafine pulverization process involves pulverizing the four mixed portions of Chinese medicinal materials using a Chinese medicine pulverizer (120 mesh), pulverizing each batch for 30 seconds, stopping for 10 seconds, repeating this process three times, and then sieving the mixture. The soaking pretreatment is as follows: add 40 parts of deionized water, let stand and soak at 25±2℃ for 2 hours, and stir with a magnetic stirrer for 1 minute each at 30 min, 60 min and 90 min to ensure that the particles completely sink and retain the soaking water; The process of the two water extractions is as follows: the extraction is carried out in two stages. For the first stage, deionized water is added to 48 parts, the temperature is kept constant at 60±2℃ for 1 hour, then gently boiled at 95-100℃ for 1.5 hours, and then filtered to obtain the filtrate. For the second stage, 32 parts of deionized water are added, the extraction parameters are repeated, and the filtrates are combined to obtain ≥40 parts. The graded filtration process is as follows: first, coarse filtration through 4 layers of sterile gauze, then filtration through a 0.22μm filter membrane until clear; if the viscosity is ≥500mPa.s, 0.1% activated carbon by weight of the filtrate is added for purification. The low-temperature concentration is: concentration at 45±2℃ and a vacuum of 0.09MPa to a relative density of 1.1-1.2 (60℃, normal pressure). The toothpaste matrix is ​​prepared by the following steps: 2.75 parts of cellulose gum are dissolved in 25 parts of deionized water at 45-50℃ and stirred until there are no particles and no layering, forming a colloid (viscosity 8000-10000 mPa.s) to obtain a cellulose gum solution for later use; 25 parts of sorbitol are dissolved in 3 parts of deionized water, and then 16.5 parts of hydrated silica, 1.25 parts of sodium lauryl sulfate, 4 parts of sodium saccharin, sodium benzoate solution (pre-dissolved in 3 parts of deionized water at 50℃ to obtain 0.4 parts of sodium benzoate), and 0.7 parts of sodium monofluorophosphate are added sequentially. The mixture is stirred for 1 minute until completely dissolved, then the prepared cellulose gum solution is added, followed by 39-41 parts of deionized water. The mixture is then stirred at 25℃ for 15 minutes to obtain a matrix suspension with a viscosity of 3000-4000 mPa.s.

2. The compound honeysuckle toothpaste according to claim 1, characterized in that, The raw materials used to prepare the toothpaste base meet the following requirements: cellulose gum viscosity ≥ 5000 mPa.s, sorbitol purity ≥ 98%, hydrated silica particle size 5-15 μm, Mohs hardness ≤ 3, sodium lauryl sulfate purity ≥ 95%, sodium saccharin and sodium benzoate purity ≥ 99%, sodium monofluorophosphate is toothpaste industrial grade, conforms to GB24567-2009 requirements, purity ≥ 98.0%, total fluoride in the finished product is controlled at 0.05%-0.15%, and deionized water conductivity ≤ 10 μS / cm, pH 6.5-7.

5.

3. A method for preparing the compound honeysuckle toothpaste according to claim 1, comprising the following steps: S1. Preparation of Chinese herbal extracts: By weight, 1.5 parts of honeysuckle, 1 part of angelica dahurica, 1 part of bletilla striata, and 0.5 parts of licorice, totaling 4 parts, are mixed and ultra-finely pulverized, then soaked, extracted twice with water, graded and filtered, and concentrated at low temperature to obtain a Chinese herbal concentrate. The ultrafine pulverization process involves mixing four portions of Chinese medicinal herbs, pulverizing them using a Chinese medicine pulverizer (120 mesh), pulverizing each batch for 30 seconds, stopping for 10 seconds, repeating this process three times, and then sieving. The soaking pretreatment is as follows: add 40 parts of deionized water, let stand and soak at 25±2℃ for 2 hours, and stir with a magnetic stirrer for 1 minute each at 30 min, 60 min and 90 min to ensure that the particles completely sink. The process of the two water extractions is as follows: the extraction is carried out in two stages. For the first stage, deionized water is added to 48 parts, the temperature is kept constant at 60±2℃ for 1 hour, then gently boiled at 95-100℃ for 1.5 hours, and then filtered to obtain the filtrate. For the second stage, 32 parts of deionized water are added, the extraction parameters are repeated, and the filtrates are combined to obtain ≥40 parts. The graded filtration process is as follows: first, coarse filtration through 4 layers of sterile gauze, then filtration through a 0.22μm filter membrane until clear; if the viscosity is ≥500mPa.s, 0.1% activated carbon by weight of the filtrate is added for purification. The low-temperature concentration is carried out at 45±2℃ and a vacuum of 0.09MPa until the relative density is 1.1-1.2 (60℃, normal pressure). 4.S2, Toothpaste matrix preparation: Dissolve 2.75 parts of cellulose gum in 25 parts of deionized water at 45-50℃ and stir until there are no particles and no layering, forming a colloid (viscosity 8000-10000 mPa.s) to obtain a cellulose gum solution for later use; dissolve 25 parts of sorbitol in 3 parts of deionized water, then add 16.5 parts of hydrated silica, 1.25 parts of sodium lauryl sulfate, 4 parts of sodium saccharin, sodium benzoate solution (pre-dissolved in 3 parts of deionized water at 50℃ to obtain 0.4 parts of sodium benzoate), and 0.7 parts of sodium monofluorophosphate in sequence, stir for 1 minute until completely dissolved, then add the prepared cellulose gum solution, then add 39-41 parts of deionized water, and stir at 25℃ for 15 minutes to obtain a matrix suspension with a viscosity of 3000-4000 mPa.s; S3. Mixing and homogenization: The Chinese herbal concentrate at 45℃ was added to the matrix suspension in three portions and stirred at 200r / min for 15min. The viscosity was measured to be 5000-8000mPa.s. The mixture was then transferred to a homogenizer and homogenized at 12000r / min for 10min. The cup wall was scraped at the 3rd and 6th minutes to ensure that there were no particles ≥50μm and no stratification, thus obtaining the compound honeysuckle toothpaste.

5. The preparation method according to claim 3, characterized in that, The raw materials for preparing the toothpaste matrix in step S2 meet the following requirements: cellulose gum viscosity ≥ 5000 mPa·s, sorbitol purity ≥ 98%, hydrated silica particle size 5–15 μm, Mohs hardness ≤ 3, sodium lauryl sulfate purity ≥ 95%, sodium saccharin and sodium benzoate purity ≥ 99%, sodium monofluorophosphate is toothpaste industrial grade, conforms to GB24567-2009 requirements, purity ≥ 98.0%, total fluoride in the finished product is controlled at 0.05%–0.15%, deionized water conductivity ≤ 10 μS / cm, pH 6.5–7.

5.

6. The compound honeysuckle toothpaste according to claim 1 or 2 or the compound honeysuckle toothpaste prepared by the preparation method according to claim 3 or 4, in oral care, or in the preparation of oral care products, or in the preparation of products or drugs for the prevention and treatment of ulcers and dental caries.

7. An extract from a traditional Chinese medicine, characterized in that, The following preparation method was used to prepare the following: by weight, 1.5 parts of honeysuckle, 1 part of angelica, 1 part of bletilla, and 0.5 parts of licorice were prepared, totaling 4 parts. The medicinal materials were mixed and ultra-finely pulverized, pretreated by soaking, extracted twice with water, graded and filtered, and concentrated at low temperature to obtain the Chinese medicine concentrate. The ultrafine pulverization process involves pulverizing the four mixed portions of Chinese medicinal materials using a Chinese medicine pulverizer (120 mesh), pulverizing each batch for 30 seconds, stopping for 10 seconds, repeating this process three times, and then sieving the mixture. The soaking pretreatment is as follows: add 40 parts of deionized water, let stand and soak at 25±2℃ for 2 hours, and stir with a magnetic stirrer for 1 minute each at 30 min, 60 min and 90 min to ensure that the particles completely sink and retain the soaking water; The process of the two water extractions is as follows: the extraction is carried out in two stages. For the first stage, deionized water is added to 48 parts, the temperature is kept constant at 60±2℃ for 1 hour, then gently boiled at 95-100℃ for 1.5 hours, and then filtered to obtain the filtrate. For the second stage, 32 parts of deionized water are added, the extraction parameters are repeated, and the filtrates are combined to obtain ≥40 parts. The graded filtration process is as follows: first, coarse filtration through 4 layers of sterile gauze, then filtration through a 0.22μm filter membrane until clear; if the viscosity is ≥500mPa.s, 0.1% activated carbon by weight of the filtrate is added for purification. The low-temperature concentration is carried out at 45±2℃ and a vacuum of 0.09MPa until the relative density is 1.1-1.2 (60℃, normal pressure).

8. The use of the Chinese herbal extract according to claim 6 in oral care, or in the preparation of oral care products, or in the preparation of products or drugs for the prevention and treatment of ulcers and dental caries.

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