Agilawood combined extract and application thereof in oral care
By scientifically combining extracts of agarwood, lavender, Panax notoginseng, and Scutellaria baicalensis, and using supercritical fluid extraction and molecular distillation techniques, a stable oral care composition is prepared. This solves the problem of poor treatment effects for oral ulcers, achieving multi-stage treatment and improved stability, and is suitable for products such as toothpaste.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-26
- Publication Date
- 2026-03-31
AI Technical Summary
In the existing technology, single agarwood extract has limited efficacy in treating oral ulcers with complex causes and is costly. There is a lack of systematic and in-depth research on the combination of multiple Chinese herbal extracts in oral care, resulting in unstable product efficacy or difficulty in large-scale production.
A combination of extracts from agarwood, lavender, Panax notoginseng, and Scutellaria baicalensis was used to prepare agarwood extract through supercritical fluid extraction and molecular distillation. Agarwood extract was then mixed with lavender, Panax notoginseng, and Scutellaria baicalensis extracts using polysorbate 60 as an emulsifier to form a stable oral care composition suitable for products such as toothpaste.
It achieves multi-stage treatment of oral ulcers, with better results than single-ingredient or simple compound formulas. The composition has good stability, is suitable for a variety of oral care products, has high safety, and can effectively inhibit oral pathogens, reduce inflammation, and promote ulcer healing.
Smart Images
Figure CN121754464A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of oral care technology, and in particular to an agarwood extract and its application in oral care. Background Technology
[0002] Oral health is an important component of overall health. Oral ulcers, a common oral mucosal disease, have a high incidence rate and are prone to recurrence. Agarwood, a traditional and precious medicinal material, has the effects of regulating qi and relieving pain, warming the stomach and stopping vomiting, and calming asthma. Modern pharmacological research shows that agarwood volatile oil and its extracts are rich in sesquiterpenes, chromones, and other active ingredients, possessing various biological activities such as anti-inflammatory, antioxidant, antibacterial, sedative, and immunomodulatory effects. This provides a theoretical basis for its adjunctive treatment of inflammatory diseases, including oral mucosal inflammation. However, the efficacy of single agarwood extracts in treating oral ulcers with complex causes may be limited, and the cost is high.
[0003] Lavender extract is renowned for its anti-inflammatory, antibacterial, and nerve-soothing properties; Panax notoginseng extract is known for its blood-activating, swelling-reducing, pain-relieving, and tissue-repairing effects; and Scutellaria baicalensis extract is widely used for its powerful anti-inflammatory, antibacterial, and antiviral activities. How to scientifically combine these synergistically potential natural active ingredients and overcome the problems of poor water solubility and instability of plant extracts to develop a stable composition that can be integrated into daily oral care routines and effectively target multiple pathological aspects of oral ulcers (anti-inflammatory, analgesic, antibacterial, and healing-promoting effects) has become a pressing technical problem in this field.
[0004] While there are reports of using various Chinese herbal extracts in oral care, existing technologies mostly focus on simple mixing. There is a lack of systematic and in-depth research on the optimization of extraction processes for core active ingredients (such as agarwood), the precise proportions and synergistic relationships between components, and the stabilization treatment of the final composition in complex oral care matrices. This results in unstable product efficacy or difficulty in large-scale production. Summary of the Invention
[0005] The purpose of this invention is to address the problems existing in the prior art by proposing an agarwood compound extract and its application in oral care.
[0006] To achieve the above objectives, the present invention adopts the following technical solution: An agarwood extract, by weight percentage, comprises the following components: Agarwood extract 5%–10%; Lavender extract 15%–20%; 15%–25% Panax notoginseng root extract; Scutellaria baicalensis extract 15%–25%; Surfactants 5%–8%; Soothing and anti-allergic agents 0.5%–1%; And the remaining water-based matrix; The surfactant is polysorbate 60, the soothing and anti-allergic agent is dipotassium glycyrrhizate, and the aqueous matrix is deionized water.
[0007] As a preferred embodiment, the agarwood extract contains sesquiterpenoids and chromones derived from agarwood; The lavender extract contains linalool and flavonoids; The Panax notoginseng root extract contains notoginsenosides; the Scutellaria baicalensis extract contains baicalin.
[0008] As a preferred embodiment, the agarwood extract is prepared by a method comprising the following steps: S1. Raw material pretreatment: The agarwood raw material is cleaned and then pulverized at low temperature until it passes through an 80-mesh sieve to obtain agarwood powder; S2. Supercritical fluid extraction: The agarwood powder is placed in a supercritical carbon dioxide extraction device and extracted under a dynamic pressure gradient and in the presence of an entrainer to obtain a crude extract. S3. Molecular distillation purification: The crude extract is subjected to two-stage gradient molecular distillation, and the distillation products are collected to obtain the agarwood extract.
[0009] As a preferred embodiment, in step S1, the cryogenic pulverization is carried out with the assistance of liquid nitrogen, and the pulverization environment temperature is maintained at -30°C to -25°C; the agarwood powder is then dried to constant weight under vacuum conditions at 40°C to 50°C.
[0010] As a preferred embodiment, in step S2, the dynamic pressure gradient is as follows: extraction begins at an initial pressure of 18±0.5MPa, is maintained for 0.5 to 1 hour, then the pressure is reduced to 16±0.5MPa to continue extraction, and in the last 30 minutes before the end of extraction, the pressure is increased back to 17±0.5MPa. The entrainer is anhydrous ethanol, accounting for 0.5% to 1.0% of the total carbon dioxide flow rate; the extraction temperature is controlled at 40℃±2℃.
[0011] As a preferred embodiment, in step S2, the flow rate of supercritical carbon dioxide is 300-310 L / h; after extraction, the crude extract is collected under the conditions of separation pressure 6±0.5 MPa and separation temperature 35℃±2℃.
[0012] As a preferred embodiment, in step S3, the conditions for the second-order gradient molecular distillation are as follows: First-stage distillation: system absolute pressure 40-60 Pa, distillation temperature 75-85℃, scraper rotation speed 200-300 rpm; Two-stage distillation: system absolute pressure ≤10Pa, distillation temperature 115~125℃, scraper rotation speed 150~250rpm; Before the material enters the distillation system, it is preheated at 80℃±5℃.
[0013] A method for preparing agarwood compound extract includes the following mixing and emulsification steps: The lavender extract, Panax notoginseng root extract, and Scutellaria baicalensis extract were premixed at room temperature to form a first mixture; The first mixture was transferred to a homogenizing emulsification device, and the agarwood extract, polysorbate 60, dipotassium glycyrrhizate and deionized water were added in sequence. The agarwood extract was dispersed and emulsified at a temperature of 50℃±10℃ and a rotation speed of 2000~3000rpm until the system was homogeneous and stable.
[0014] An oral care composition comprising an effective amount of agarwood extract and an oral care acceptable carrier; The agarwood extract is present in the oral care composition at a weight percentage of 0.1% to 20%, preferably 1% to 10%. When the oral care composition is toothpaste, it comprises the following components: 20%–50% abrasive, 10%–30% humectant, 0.5%–2.5% foaming agent, 0.1%–2% binder, 0.1%–0.5% sweetener, 0.01%–0.5% preservative, agarwood extract, and the balance being water.
[0015] The application of an agarwood extract and an oral care composition in the preparation of products for the prevention and treatment of oral mucosal damage; The oral mucosal lesions are recurrent aphthous ulcers, traumatic ulcers, or inflammation-related oral mucositis.
[0016] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention scientifically combines extracts from four plants: agarwood, lavender, Panax notoginseng, and Scutellaria baicalensis. Agarwood and lavender exert anti-inflammatory, analgesic, and soothing effects; Panax notoginseng promotes blood circulation and removes blood stasis, improves local microcirculation in ulcers, and promotes granulation tissue growth; Scutellaria baicalensis has strong broad-spectrum antibacterial and antiviral effects, and controls secondary infections. The four ingredients work synergistically to exert a comprehensive effect from multiple aspects such as anti-inflammatory, analgesic, antibacterial, and healing-promoting effects. This approach targets the complex pathological mechanism of oral ulcers and is more effective than single-ingredient or simple compound formulas.
[0017] 2. By introducing polysorbate 60 as an emulsifier, this invention successfully stabilizes multiple fat-soluble and water-soluble extracts in the same aqueous system, solving the problem of easy precipitation and stratification of plant compound extracts. The resulting combined extract has uniform and stable properties and is well compatible with various oral care product bases (such as toothpaste paste and mouthwash solution), making it easy to add and expanding its application range.
[0018] 3. All ingredients in this invention are derived from natural plants or recognized safe cosmetic / pharmaceutical excipients. They do not contain antibiotics, hormones, or other chemical drugs that may cause side effects or drug resistance. They are highly safe for long-term use. The addition of dipotassium glycyrrhizate further enhances the product's soothing and anti-allergic properties and reduces potential irritation to sensitive oral mucosa. Attached Figure Description
[0019] Figure 1 This is a flowchart illustrating the overall process for preparing an agarwood extract proposed in this invention. Figure 2 Comparative images of representative macroscopic morphology of oral ulcers in SD rats from different groups after drug administration at different times. Detailed Implementation
[0020] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.
[0021] It should be understood that, when used in this specification and the appended claims, the terms "comprising" and "including" indicate the presence of the described features, integrals, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components and / or collections thereof.
[0022] It should also be understood that the terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. As used in this specification and the appended claims, the singular forms “a,” “an,” and “the” are intended to include the plural forms unless the context clearly indicates otherwise.
[0023] It should also be further understood that the term "and / or" as used in this specification and the appended claims refers to any combination of one or more of the associated listed items and all possible combinations, and includes such combinations.
[0024] Example, refer to Figures 1 to 2This invention provides an agarwood extract with oral care benefits, comprising the following components by weight percentage: Agarwood extract 5%–10%; lavender extract 15%–20%; Panax notoginseng root extract 15%–25%; Scutellaria baicalensis extract 15%–25%; surfactant 5%–8%; soothing and anti-allergic agent 0.5%–1%; and the balance being an aqueous matrix; The surfactant is polysorbate 60, the soothing and anti-allergic agent is dipotassium glycyrrhizate, and the aqueous matrix is deionized water.
[0025] It is worth noting that agarwood extract contains sesquiterpenoids (such as agaric spirol and agaric aldehyde) and chromones (such as furano-agaric aldehyde and 2-(2-phenylethyl)chromone) derived from agarwood; lavender extract contains linalool and flavonoids; Panax notoginseng root extract contains Panax notoginseng saponins (such as ginsenosides Rg1 and Rb1); and Scutellaria baicalensis extract contains baicalin.
[0026] This invention provides a method for preparing the above-mentioned agarwood extract, which includes the following steps: S1. Raw material pretreatment: The agarwood raw material is cleaned and then pulverized at low temperature until it passes through an 80-mesh sieve to obtain agarwood powder; S2. Supercritical fluid extraction: Agarwood powder is placed in a supercritical carbon dioxide extraction device and extracted under dynamic pressure gradient and in the presence of entrainer to obtain crude extract. S3. Molecular distillation purification: The crude extract is subjected to two-stage gradient molecular distillation, and the distillation products are collected to obtain agarwood extract.
[0027] Furthermore, in step S1, cryogenic pulverization is carried out with the assistance of liquid nitrogen, and the pulverization environment temperature is maintained at -30℃ to -25℃ to prevent thermal degradation of the active ingredients. The pulverized powder is then dried to constant weight under vacuum conditions at 40℃ to 50℃.
[0028] In step S2, the dynamic pressure gradient is as follows: extraction begins at an initial pressure of 18±0.5 MPa, is maintained for 0.5–1 hour, then the pressure is reduced to 16±0.5 MPa to continue extraction. In the last 30 minutes before the end of extraction, the pressure is increased back to 17±0.5 MPa. This gradient design aims to preferentially extract readily soluble components and then improve the selectivity for some poorly soluble target components through a depressurization-increase process. Anhydrous ethanol, comprising 0.5%–1.0% of the total carbon dioxide flow rate, is used to improve the yield of polar components. The extraction temperature is controlled at 40℃±2℃, and the supercritical carbon dioxide flow rate is 300–310 L / h. After extraction, the crude extract is collected under separation pressure of 6±0.5 MPa and separation temperature of 35℃±2℃.
[0029] In step S3, the conditions for the two-stage gradient molecular distillation are as follows: First-stage distillation: system absolute pressure 40–60 Pa, distillation temperature 75–85 °C, scraper rotation speed 200–300 rpm, mainly removing light component impurities; Second-stage distillation: system absolute pressure ≤10 Pa, distillation temperature 115–125 °C, scraper rotation speed 150–250 rpm, under which the target active component is efficiently separated and collected. Before entering the distillation system, the material is preheated at 80 °C ± 5 °C to reduce viscosity.
[0030] This invention provides a method for preparing the above-mentioned agarwood compound extract, comprising a mixing and emulsification step: Lavender extract, Panax notoginseng root extract and Scutellaria baicalensis extract were premixed at room temperature to form a first mixture; The first mixture was transferred to a homogenizing emulsifier, and agarwood extract, polysorbate 60, dipotassium glycyrrhizate and deionized water were added in sequence. The agarwood extract was dispersed and emulsified at 50℃±10℃ and a rotation speed of 2000~3000rpm until the system was homogeneous and stable. This step ensured that the fat-soluble active ingredients were fully emulsified by polysorbate 60, forming a stable O / W microemulsion or nanoemulsion system, which is beneficial for subsequent applications.
[0031] This invention provides an oral care composition comprising an effective amount of the above-described agarwood extract and an oral care acceptable carrier. The weight percentage of the agarwood extract in the oral care composition is preferably 0.1% to 20%, more preferably 1% to 10%.
[0032] Oral care compositions may be formulated into any dosage form acceptable in the art, including but not limited to toothpaste, mouthwash, oral spray, oral lozenges, oral gels or oral patches.
[0033] When the oral care composition is toothpaste, its typical components may include: abrasives (such as hydrated silica, 20%–50%), humectants (such as sorbitol and glycerin, 10%–30%), foaming agents (such as sodium lauryl sulfate, 0.5%–2.5%), binders (such as sodium carboxymethyl cellulose and xanthan gum, 0.1%–2%), sweeteners (such as sodium saccharin, 0.1%–0.5%), preservatives (such as sodium benzoate, 0.01%–0.5%), and the above-mentioned agarwood extract, with the balance being water.
[0034] This invention provides the use of the above-mentioned agarwood extract or oral care composition in the preparation of products for the prevention and / or treatment of oral mucosal damage; Oral mucosal damage includes, but is not limited to, recurrent aphthous ulcers, traumatic ulcers, or inflammation-related stomatitis. The product has one or more of the following effects: inhibiting oral pathogens (such as Porphyromonas gingivalis, Streptococcus mutans, etc.), reducing oral inflammation, relieving oral pain, promoting oral ulcer healing, and reducing bad breath.
[0035] Preparation Example 1 of the Invention: Preparation of Agarwood Extract Step 1: Take 500g of imported Malaysian agarwood blocks and ultrasonically wash them three times with deionized water for 5 minutes each time to thoroughly remove surface impurities. Place the washed agarwood raw material into an ultrafine pulverizer and purge it with liquid nitrogen to maintain the pulverizing chamber temperature at -30℃ for low-temperature embrittlement pulverization. After pulverization, pass the material through an 80-mesh standard sieve and collect the undersized powder. Place the powder in a vacuum drying oven and dry it at 40℃ and -0.09MPa for 6 hours to obtain dried agarwood powder for later use.
[0036] Step 2: Load approximately 300g of the above-mentioned agarwood powder into the 1L extraction vessel of an E420-40-48 type supercritical CO2 extraction apparatus. Set the extraction temperature to 40℃, the separation vessel I temperature to 35℃, and the pressure to 6MPa. Open the CO2 cylinder, adjust the flow rate to 306L / h, and start the entrainer pump, pumping in food-grade anhydrous ethanol as an entrainer at a flow rate of 0.5%. Use a dynamic pressure gradient: first increase the pressure to 18MPa to start extraction and maintain it for 1 hour; then slowly decrease the pressure to 16MPa and continue extraction for 30 minutes; in the last 30 minutes, gradually increase the pressure back to 17MPa. The total extraction time is 2 hours. Collect approximately 12.5g of dark brown, oily crude agarwood extract from the outlet of the separation vessel.
[0037] Step 3: Inject the crude extract into an FZL-001 short-path molecular distillation apparatus. Set the first-stage distillation conditions: system absolute pressure 50 Pa, distillation temperature 80℃, scraper rotation speed 250 rpm, preheater temperature 80℃. After removing light components by the first-stage distillation, collect the middle fraction for the second-stage distillation. Second-stage distillation conditions: system absolute pressure 8 Pa, distillation temperature 120℃, scraper rotation speed 200 rpm. In the receiver of the second-stage distillation fraction, collect approximately 9.8 g of a yellowish-brown, clear, oily agarwood extract with a rich agarwood characteristic aroma. HPLC analysis showed that the total content of characteristic sesquiterpenes and 2-(2-phenylethyl)chromones was significantly higher than that of the extract obtained by conventional alcohol extraction.
[0038] Example 1: Preparation of Agarwood Combination Extract Weigh each raw material according to the following weight percentages: Agarwood extract (prepared from Preparation Example 1) 10%, lavender oil extract (purchased from a plant extraction company, linalool content ≥30%) 20%, Panax notoginseng root water extract (purchased from a plant extraction company, total Panax notoginseng saponin content ≥8%) 25%, baicalin water extract (purchased from a plant extraction company, baicalin content ≥85%) 25%, polysorbate 60 8%, dipotassium glycyrrhizate 1%. Deionized water balance (calculated as 11%) Preparation method: In a mixing jar, lavender extract, Panax notoginseng root extract and Scutellaria baicalensis extract were added in sequence and stirred at 500 rpm for 15 minutes at room temperature until well mixed to obtain the first mixture.
[0039] Transfer the first mixture to a high-speed dispersion homogenizer. Turn on the heating to raise the material temperature to 50°C.
[0040] Agarwood extract, polysorbate 60, and dipotassium glycyrrhizate were added sequentially to the homogenizer.
[0041] Maintain the temperature at 50℃±2℃, start the high-speed shearing, and gradually increase the rotation speed to 2500 rpm. At this speed, slowly add the prescribed amount of deionized water.
[0042] The agarwood extract was continuously emulsified and sheared at 2500 rpm for 30 minutes until a uniform, stable, pale yellow-brown emulsion was formed.
[0043] Example 1 and Comparative Examples 1-2 The proportions of each component in Example 1 were changed, and the specific ratios are shown in Table 1. The preparation method is the same as in Example 1.
[0044] Table 1: Composition of the formulations in the examples and comparative examples (weight percentage %) The in vitro antibacterial rate of the agarwood combination extracts obtained in Example 1 and Comparative Examples 1-2 against common oral pathogens was tested.
[0045] Experimental Example 1 Antibacterial test: The antibacterial and bacteriostatic effects of the composition were tested according to the evaluation method of QB / T2738-2012. The tested bacteria were Escherichia coli, Staphylococcus aureus, Porphyromonas gingivalis, Helicobacter pylori, and Streptococcus mutans. Among them, Helicobacter pylori is a suspected pathogen of halitosis, Escherichia coli and Staphylococcus aureus are pathogens associated with oral purulent inflammation, Porphyromonas gingivalis is a suspected pathogen of periodontal inflammation and halitosis, and Streptococcus mutans is the most important pathogen of dental caries.
[0046] (1) Preparation of test bacterial suspension ① Take the freeze-dried bacterial culture, add an appropriate amount of nutrient broth using a capillary pipette, and gently blow and aspirate several times to dissolve and disperse the culture. Take a test tube containing 5.0 mL of nutrient broth medium, add a small amount of bacterial suspension, and incubate at 37℃ for 24 hours. Use an inoculation loop to take the bacterial suspension from the first generation culture, streak it onto a nutrient agar plate, and incubate at 37℃ for 24 hours. Pick typical colonies from the above second generation culture, inoculate them onto a nutrient agar slant, and incubate at 37℃ for 24 hours to obtain the third generation culture. ② Take 3-5 mL of fresh third-generation culture and add it to a test tube with a pipette. Repeatedly blow and aspirate to wash off the bacterial growth. Then, use a pipette to transfer the washing solution to another sterile test tube and mix with an electric mixer for 20 seconds, or shake it 80 times on the palm of your hand to make the bacteria evenly suspended. ③ The bacterial suspension prepared initially is roughly measured for its bacterial concentration, then diluted to the required concentration and stored in a refrigerator at 4°C for later use.
[0047] ④ Dilute the test bacterial suspension appropriately with PBS solution, and recover 1 x 10⁻⁶ bacteria. 4 ~9x10 4 cfu / mL; (2) Determination of antibacterial rate Dilute the test sample with water for injection to the specified concentration (0.01 mg / ml). Then, take 5.0 mL of the original test sample solution and place it in a sterile test tube. Incubate at 30°C for 5 min. Next, take 0.1 mL of the test bacterial solution and add it to the test tube containing 5.0 mL of the original sample solution. Mix quickly and start timing immediately. After incubation for 3 min, take 0.5 mL of the mixture and add it to a test tube containing 4.5 mL of sterile PBS. Mix thoroughly and let stand for 10 min. Then, take 1 mL of the sample solution and place it in a sterile Petri dish. Pour in 15 mL of nutrient agar medium cooled to 40°C–45°C. Rotate the Petri dish to ensure thorough mixing. After the agar solidifies, invert the Petri dish and incubate at 37°C for 48 h. Count the viable colonies and calculate the inhibition rate. Use PBS solution instead of the test sample, and follow the above steps as a control. The antibacterial performance test results are shown in Table 2. The average antibacterial rate of Example 1 against the five bacteria was higher than that of Comparative Example 1 and Comparative Example 2, indicating that Example 1 performed better in inhibiting these common bacteria.
[0048] Table 2 Results of antibacterial performance test To demonstrate the effects of different mass ratios of agarwood extracts in toothpaste, Examples 1, 1, and 2 were added to the blank toothpaste components. The blank toothpaste components in this invention were: 30% hydrated silica, 10% sorbitol, 10% glycerin, 5% butylene glycol, 1% cellulose gum, 0.2% xanthan gum, 0.4% sodium saccharin, 0.4% dicalcium phosphate dihydrate, 0.1% sodium benzoate, 0.6% flavoring, 0.01% sodium hydroxide, and the remainder being deionized water.
[0049] Experimental Example 2 Stability test The toothpaste was left to stand at room temperature for 10 weeks, and the changes in the paste were observed. The test results are shown in Table 3, indicating that both the blank toothpaste and the toothpaste with added agarwood extract have stability.
[0050] Table 3. Results of toothpaste stability test Experimental Example 3 Anti-inflammatory performance test Twenty patients with oral inflammation were selected from the hospital's dental department. They brushed their teeth with the toothpaste twice daily, morning and evening. After each use, their oral condition was re-examined at the hospital, and the effectiveness rate was calculated. The anti-inflammatory effectiveness rate was calculated as: (Number of patients with effective anti-inflammatory effect / Total number of patients) × 100%. The results are shown in Table 4. Table 4 shows that the anti-inflammatory effectiveness rates of Example 1 and Comparative Examples 1-2 of this invention are significantly higher than that of the blank toothpaste, indicating that this invention has better anti-inflammatory properties. Example 1 exhibits the best anti-inflammatory performance because of its high content of agarwood extract in the agarwood combination extract.
[0051] Table 4. Results of Anti-inflammatory Performance Tests Test Example 4 Therapeutic effect study in rat model of oral ulcer (1) Establishment of animal models A 5% solution of 50-Zephalosporin 50 was prepared with water for injection and diluted to 0.5% with physiological saline. Rats were anesthetized by intraperitoneal injection at a dose of 50 mg / kg. The rats were then fixed in a supine position on a surgical board. The oral cavity was opened with surgical forceps to expose the mandibular vestibular mucosa. The mandibular mucosa of the SD rats was dried with sterile cotton balls. Filter paper was soaked in 50% glacial acetic acid for 5 seconds, then gently applied to the target mucosa with surgical forceps for 20 seconds before removing the filter paper. The mucosa was rinsed three times with PBS buffer to remove residual acetic acid. After 48 hours, approximately circular ulcers with a diameter of 4–6 mm were observed on the mandibular mucosa of the rats.
[0052] (2) Animal grouping and administration Fifty-six rats were acclimatized for one week and then numbered and randomly divided into seven groups using a random number table: blank group, model group, positive control group, blank toothpaste group, Example 1 group, comparative example 1 group, and comparative example 2 group. Two days after modeling, the positive control group, blank toothpaste group, Example 1 group, comparative example 1 group, and comparative example 2 group were administered the drug to the ulcer site. The rats in the blank group received an equal volume of PBS buffer, and the positive control group was controlled with dexamethasone acetate oral patch (DAAT). The administration was once a day for 7 consecutive days.
[0053] (3) Measurement of ulcer area The maximum transverse diameter (D1) and maximum longitudinal diameter (D2) of the oral ulcers in rats were measured before administration and on day 7 after administration. The ulcer area (mm2) was calculated as 0.25 × ×D1(mm)×D2(mm), The value is 3.14.
[0054] (4) Histological observation Edge tissues of oral ulcers from 7 groups were collected, fixed in 4% paraformaldehyde fixative for 48 hours, routinely embedded in paraffin, serially sectioned, stained with hematoxylin and eosin (HE) and Masson staining, and then observed under a microscope after mounting.
[0055] Figure 1 Compared with the control group, the model group showed obvious typical ulcer lesions after the acetic acid method was used to create the model. Compared with the control group, the mandibular mucosa showed obvious pitting defects. The ulcers were roughly round, covered with a yellowish-white pseudomembrane, and surrounded by congestion and swelling. The results in Table 5 showed that the ulcers showed a certain degree of self-healing. As time went on, their area gradually decreased, but the overall value remained relatively large. This indicates that the natural healing process of oral ulcers in the model group rats was slow and external intervention was required to promote healing.
[0056] On day 5 of drug administration, compared with the model group, the oral ulcer area of the rats in Example 1 was significantly reduced, which was significantly better than that of Comparative Groups 1 and 2, indicating that the addition of agarwood extract can enhance its healing-promoting effect. Comparative Group 2, which did not contain agarwood extract, showed poor healing, indicating that agarwood extract plays a crucial role in the oral healing process.
[0057] Table 5 Comparison of changes in oral ulcer area among different groups of rats (x±s, mm) 2 ) Note: Compared with the blank group, ### p < 0.001; compared with the model group, *** p<0.001, ** p<0.01, * p<0.05.
[0058] Conclusion: Animal experiments show that the agarwood extract prepared in Example 1 of this invention can significantly promote the healing of experimental oral ulcers in rats, and its effect is better than that of the positive control drug (hormone) and the comparative ratio without emulsifier or without agarwood extract.
[0059] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
Claims
1. An agarwood extract, characterized in that, By weight percentage, it consists of the following components: Agarwood extract 5%–10%; Lavender extract 15%–20%; 15%–25% Panax notoginseng root extract; Scutellaria baicalensis extract 15%–25%; Surfactants 5%–8%; Soothing and anti-allergic agents 0.5%–1%; And the remaining water-based matrix; The surfactant is polysorbate 60, the soothing and anti-allergic agent is dipotassium glycyrrhizate, and the aqueous matrix is deionized water.
2. The agarwood extract according to claim 1, characterized in that, The agarwood extract contains sesquiterpenoids and chromones derived from agarwood; The lavender extract contains linalool and flavonoids; The Panax notoginseng root extract contains notoginsenosides; the Scutellaria baicalensis extract contains baicalin.
3. The agarwood extract according to claim 2, characterized in that, The agarwood extract was prepared by a method comprising the following steps: S1. Raw material pretreatment: The agarwood raw material is cleaned and then pulverized at low temperature until it passes through an 80-mesh sieve to obtain agarwood powder; S2. Supercritical fluid extraction: The agarwood powder is placed in a supercritical carbon dioxide extraction device and extracted under a dynamic pressure gradient and in the presence of an entrainer to obtain a crude extract. S3. Molecular distillation purification: The crude extract is subjected to two-stage gradient molecular distillation, and the distillation products are collected to obtain the agarwood extract.
4. The agarwood extract according to claim 3, characterized in that, In step S1, cryogenic pulverization is carried out with the assistance of liquid nitrogen, and the pulverization environment temperature is maintained at -30℃ to -25℃; the agarwood powder is then dried to constant weight under vacuum conditions at 40℃ to 50℃.
5. The agarwood extract according to claim 3, characterized in that, In step S2, the dynamic pressure gradient is as follows: extraction begins at an initial pressure of 18±0.5MPa, is maintained for 0.5 to 1 hour, then the pressure is reduced to 16±0.5MPa to continue extraction, and in the last 30 minutes before the end of extraction, the pressure is increased back to 17±0.5MPa. The entrainer is anhydrous ethanol, accounting for 0.5% to 1.0% of the total carbon dioxide flow rate; the extraction temperature is controlled at 40℃±2℃.
6. The agarwood extract according to claim 3, characterized in that, In step S2, the flow rate of supercritical carbon dioxide is 300-310 L / h; after extraction, the crude extract is collected under the conditions of separation pressure 6±0.5 MPa and separation temperature 35℃±2℃.
7. The agarwood extract according to claim 3, characterized in that, In step S3, the conditions for the second-order gradient molecular distillation are as follows: First-stage distillation: system absolute pressure 40-60 Pa, distillation temperature 75-85℃, scraper rotation speed 200-300 rpm; Two-stage distillation: system absolute pressure ≤10Pa, distillation temperature 115~125℃, scraper rotation speed 150~250rpm; Before the material enters the distillation system, it is preheated at 80℃±5℃.
8. A method for preparing an agarwood extract as described in any one of claims 1-7, characterized in that, Includes the following mixing and emulsification steps: The lavender extract, Panax notoginseng root extract, and Scutellaria baicalensis extract were premixed at room temperature to form a first mixture; The first mixture was transferred to a homogenizing emulsification device, and the agarwood extract, polysorbate 60, dipotassium glycyrrhizate and deionized water were added in sequence. The agarwood extract was dispersed and emulsified at a temperature of 50℃±10℃ and a rotation speed of 2000~3000rpm until the system was homogeneous and stable.
9. An oral care composition, characterized in that, It contains an effective amount of the agarwood complex extract as described in any one of claims 1-7, and an oral care acceptable carrier; The agarwood extract is present in the oral care composition at a weight percentage of 0.1% to 20%, preferably 1% to 10%. When the oral care composition is toothpaste, it comprises the following components: 20%–50% abrasive, 10%–30% humectant, 0.5%–2.5% foaming agent, 0.1%–2% binder, 0.1%–0.5% sweetener, 0.01%–0.5% preservative, and agarwood extract as described in any one of claims 1-7, with the balance being water.
10. The use of an agarwood extract as described in any one of claims 1-7 and the oral care composition as described in claim 9 in the preparation of a product for the prevention and treatment of oral mucosal damage; The oral mucosal lesions are recurrent aphthous ulcers, traumatic ulcers, or inflammation-related oral mucositis.