A forsythia leaf extract, a preparation method thereof, and an application thereof

Abstract

The application relates to the technical field of plant extracts, and discloses a forsythia suspense leaf extract and application thereof. The preparation method of the forsythia suspense leaf extract is as follows: (1) forsythia suspense leaves are treated by killing green, drying and crushing, and then sprayed with a sodium hydroxide-ethanol solution and sealed and placed, followed by drying and steam explosion to obtain solid A; (2) solid A is extracted by refluxing with an ethanol solution, and then subjected to solid-liquid separation and concentration to obtain concentrated solution A, anhydrous ethanol and an additive are added into the concentrated solution A, stirred, placed, subjected to solid-liquid separation, concentrated into a paste, and then water is added into the paste, mixed, and concentrated to obtain concentrated solution B; (3) concentrated solution B is placed at room temperature, subjected to solid-liquid separation, and the collected solid is dried to obtain the forsythia suspense leaf extract. The preparation method of the forsythia suspense leaf extract in the application can effectively extract forsythoside in the forsythia suspense leaves, and the content of forsythoside in the extract can reach more than 60%.

Description

Technical Field

[0001] This invention relates to the field of plant extract technology, and more specifically, to a forsythia leaf extract and its applications. Background Technology

[0002] Forsythia suspensa, the fruit of the Forsythia plant (family Oleaceae), is a deciduous shrub belonging to the genus Forsythia. Its dried fruit has been used as a major medicinal material for over 2000 years, documented as early as the *Illustrated Materia Medica*, and is hailed as a "holy medicine for sores." In my country, Forsythia is mainly found wild, distributed in Shanxi, Shaanxi, Hubei, Shandong, Hebei, Anhui, and Henan provinces. Currently, over 230 compounds have been isolated from Forsythia, primarily forsythoside A, forsythoside A, and forsythoside B. Forsythia leaves are abundant and contain essentially the same chemical components as the fruit, with some components even present in higher concentrations. In traditional Chinese medicine, tender Forsythia leaves are often processed into health teas. Studies have confirmed that Forsythia leaves have hepatoprotective, lipid-lowering, antibacterial, antioxidant, and anti-aging effects. Wang Tingting et al. [Study on the antibacterial and anti-inflammatory activity of Forsythia suspensa and its leaves and its main chemical components [J]. Chinese Journal of Drugs and Clinical Use, 2019, 19(14):2380-2381] found that Forsythia suspensa leaves have a therapeutic effect on chronic inflammation, and the content of forsythoside in the leaves is higher than that in the fruit.

[0003] In recent years, many extraction processes for forsythosides have been developed, such as ultrasound-assisted extraction and microwave-assisted extraction. However, ultrasound-assisted extraction is costly and causes environmental pollution, while microwave-assisted extraction is unsuitable for large-scale industrial production. Therefore, there is an urgent need for a simple and efficient method to separate forsythosides from forsythia leaves. Summary of the Invention

[0004] To address the problems and shortcomings of existing technologies, this invention provides a forsythia leaf extract and its applications.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] In a first aspect, the present invention provides a method for preparing Forsythia leaf extract, comprising the following steps:

[0007] (1) The leaves of Forsythia are blanched, dried and pulverized to obtain Forsythia leaf powder; sodium hydroxide-ethanol solution is sprayed onto the Forsythia leaf powder, and then sealed and left to stand for 12-24 hours. After the sealed and left to stand treatment, the leaves are dried and steam-exploded in sequence to obtain solid A.

[0008] (2) Extract solid A by reflux with ethanol solution, then perform solid-liquid separation to obtain filtrate A; concentrate filtrate A to obtain concentrate A, add anhydrous ethanol and auxiliary agent to concentrate A, stir at 50-60℃ for 20-30 min, then let stand, and after standing, perform solid-liquid separation to obtain filtrate B; concentrate filtrate B to a paste, add water to it, mix well to obtain a mixture, concentrate the mixture to obtain concentrate B;

[0009] (3) Let the concentrated solution B stand at room temperature for 5 to 10 hours, then perform solid-liquid separation, collect the solid, and dry it to obtain the forsythia leaf extract.

[0010] Further, the preparation method of the auxiliary agent in step (2) is as follows: diatomaceous earth is added to an acidic solution and mixed, heated to boiling and then filtered to obtain acidic diatomaceous earth; the acidic diatomaceous earth is washed and added to an alkaline solution and mixed, heated to boiling and then filtered to obtain alkaline diatomaceous earth; the alkaline diatomaceous earth is washed and then mixed with dextran gel, ground and activated to obtain the auxiliary agent.

[0011] Furthermore, the mass ratio of the dextran gel to diatomaceous earth is 1:(30-60); the dextran gel is any one of G10, G50, and G100.

[0012] Furthermore, the acidic solution is a hydrochloric acid solution with a mass fraction of 10% to 15%, and the alkaline solution is a sodium hydroxide solution with a mass fraction of 2% to 5%.

[0013] Furthermore, the diatomaceous earth boils for 40–60 minutes in an acidic solution and for 30–40 minutes in an alkaline solution.

[0014] Furthermore, the activation temperature is 100–120°C, and the activation time is 10–15 min.

[0015] Further, in step (1), the ratio of the forsythia leaf powder to the sodium hydroxide-ethanol solution is 100g:(15-25)ml; the sodium hydroxide content in the sodium hydroxide-ethanol solution is 0.2-0.5g / L; the steam explosion pressure is 0.9-2.0MPa, and the time is 110-200s.

[0016] Further, in step (2), the material-to-liquid ratio of the reflux extraction is 1g:(7-11)ml, and the extraction time is 1-3h; the volume ratio of the concentrated solution A to anhydrous ethanol is 1:(2-3), and the mass ratio of the auxiliary agent to solid A is 1:(7-10).

[0017] Furthermore, the forsythia leaves mentioned in step (1) are forsythia leaves from before September.

[0018] Furthermore, the blanching in step (1) is steam blanching at a temperature of 230-250°C until the moisture content is 45-55%.

[0019] Furthermore, the drying temperature in step (1) is 40-50°C, and the product is dried to a moisture content of 8%-10%.

[0020] Further, the material described in step (1) is pulverized to 20-40 mesh.

[0021] Furthermore, the drying temperature in step (1) is 55-60°C, and the product is dried to a moisture content of 6%-8%.

[0022] Furthermore, the ethanol solution in step (2) has a mass fraction of 90% to 95%.

[0023] Furthermore, the static treatment temperature in step (2) is 25-35°C and the time is 30-60 min.

[0024] Furthermore, in step (2), the ratio of solid A to water is 1g:(1.5~2.2)ml.

[0025] Further, in step (2), the concentrated liquid A is 20% to 30% of the volume of the filtrate A, and the concentrated liquid B is 45% to 55% of the volume of the mixed liquid.

[0026] Furthermore, the drying temperature in step (3) is below 50°C, and the product is dried to a moisture content of 3% to 5%.

[0027] In a second aspect, the present invention provides a forsythia leaf extract prepared by the method described in the first aspect above.

[0028] Thirdly, the present invention provides the application of the forsythia leaf extract described in the second aspect in toothpaste.

[0029] Fourthly, the present invention provides a toothpaste comprising the forsythia leaf extract described in the second aspect above.

[0030] Further, the toothpaste, by mass fraction, comprises the following ingredients: 15% sorbitol, 12.5% ​​hydrated silica, 2% sodium lauryl sulfate, 4.22% polyethylene glycol 400, 8% glycerin, 1.5% CMC, 0.3% sodium saccharin, 3.8% forsythia leaf extract, 52.5% water, 0.05% potassium sorbate, and 0.13% sodium fluoride.

[0031] Furthermore, the water in question is purified water.

[0032] Furthermore, the forsythia leaf extract contains more than 60% forsythoside.

[0033] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0034] 1. In this invention, ethanol and polysaccharides can form a colloid, and the addition of an auxiliary agent helps to separate polysaccharide substances. Diatomaceous earth is first treated with acid to wash away inorganic salts and other impurities, and then treated with alkali to tightly bind with dextran gel. Dextran gel contains hydroxyl groups and other groups, which have an adsorption effect on non-target components such as polysaccharides. The auxiliary agent obtained by combining diatomaceous earth and dextran gel has a good adsorption effect on both polysaccharides and their gels, improving the removal of polysaccharides and other molecules, and helping to increase the content of the target substance forsythoside in the extract. Due to the adsorption effect of the auxiliary agent, some insoluble substances are separated from soluble substances to a certain extent by adsorption, which can improve the yield of forsythoside. In addition, after the auxiliary agent adsorbs polysaccharides, due to its own filter aid properties, the filtration separation is highly efficient and will not cause clogging of filter paper or filter cloth, affecting the operation.

[0035] 2. In this invention, a sodium hydroxide-ethanol solution is sprayed onto the surface of Forsythia leaf powder. Ethanol, as a solvent, can dissolve a certain amount of sodium hydroxide. Furthermore, ethanol has strong penetrating power and is easily volatile, which is conducive to forming a weak alkaline adsorption layer on the surface of Forsythia leaf powder. During steam explosion, it is easier to achieve the degradation of cellulose, lignin, etc., and release the target low molecular weight effective components.

[0036] 3. This invention uses steam explosion technology to process forsythia leaves, instantly releasing the steam molecules that have penetrated into the plant tissue. This converts the internal energy of the steam into mechanical energy, which acts on the intercellular layers of biomass tissue, promoting the release of effective components and facilitating the extraction of forsythosides from forsythia leaves.

[0037] 4. This invention provides a simple process for extracting and separating forsythosides from forsythia leaves with high raw material utilization, and the forsythoside content in the extract can reach more than 60%.

[0038] 5. The toothpaste prepared in this invention contains forsythia extract, and the forsythoside content in the extract reaches more than 50%. Forsythia extract has antiviral and antibacterial activity, which makes the forsythia toothpaste have obvious antibacterial and antiviral effects. It can effectively and quickly restore oral health for patients with oral bacterial and viral inflammation. Detailed Implementation

[0039] To make the objectives, technical solutions, and advantages of this invention clearer and more explicit, the invention is further described in detail below through embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

[0040] (I) Experiment on the exploration of adjuvants

[0041] Example 1:

[0042] A method for preparing Forsythia leaf extract, the specific steps of which are as follows:

[0043] (1) Forsythia leaves grown before September were steamed at 245℃ until the moisture content was 45%, then dried at 40℃ until the moisture content was 8%, and then pulverized to 40 mesh to obtain Forsythia leaf powder. Sodium hydroxide-ethanol solution (sodium hydroxide content was 0.4g / L, and the ratio of sodium hydroxide-ethanol solution to Forsythia leaf powder was 20ml:100g) was evenly sprayed on the Forsythia leaf powder, and then sealed and left to stand for 20h. After the sealing and standing treatment was completed, it was dried at 58℃ until the moisture content was 6%, and then steam explosion was performed. The explosion pressure was 1.5Mpa and the time was 180s to obtain solid A.

[0044] (2) Solid A was extracted by reflux for 2.5 h with 92% ethanol solution. The ratio of solid A to ethanol solution was 1 g: 10 ml. Then, solid-liquid separation was performed to obtain filtrate A. Filtrate A was concentrated to 25% of its original volume to obtain concentrate A. Anhydrous ethanol (volume ratio of concentrate A to concentrate A was 2.5:1) and auxiliary agent (mass ratio of solid A to 1:9) were added to concentrate A. The mixture was stirred at 58 °C for 25 min. Then, it was cooled to 30 °C and allowed to stand for 50 min. After the standing treatment, solid-liquid separation was performed to obtain filtrate B. Filtrate B was concentrated to a paste. Then, pure water (volume ratio of solid A to 2 ml: 1 g) was added to it and mixed well to obtain a mixture. The mixture was concentrated to 50% of its original volume to obtain concentrate B.

[0045] (3) Let the concentrated solution B cool to room temperature and stand for 8 hours, then perform solid-liquid separation, collect the solid, and dry it at 45°C until the water content is 3% to obtain the Forsythia leaf extract.

[0046] In step (2), the preparation method of the additive is as follows: diatomaceous earth is added to a 13% hydrochloric acid solution and mixed, heated to boiling for 50 minutes, and then filtered to obtain acidic diatomaceous earth. After washing away the residual hydrochloric acid in the acidic diatomaceous earth, it is added to a 3% sodium hydroxide solution and mixed, heated to boiling for 35 minutes, and then filtered to obtain alkaline diatomaceous earth. After washing away the residual sodium hydroxide in the alkaline diatomaceous earth, dextran gel G50 and diatomaceous earth are mixed and ground at a mass ratio of 1:50, and then activated at 110°C for 13 minutes to obtain the additive.

[0047] Comparative Example 1

[0048] Comparative Example 1 is basically the same as Example 1, except that no additives are added in step (2).

[0049] Comparative Example 2

[0050] Comparative Example 2 is basically the same as Example 1, except that in step (2), the preparation method of the additive is as follows: add diatomaceous earth to a sodium hydroxide solution with a mass fraction of 3% and mix well, heat to boiling for 35 minutes, then filter to obtain alkaline diatomaceous earth, wash the residual sodium hydroxide in the alkaline diatomaceous earth, mix dextran gel G50 and diatomaceous earth at a mass ratio of 1:50, grind, and then activate at 110°C for 13 minutes to obtain the additive.

[0051] Comparative Example 3

[0052] Comparative Example 3 is basically the same as Example 1, except that in step (2), the preparation method of the additive is as follows: diatomaceous earth is added to a 13% hydrochloric acid solution and mixed, heated to boiling for 50 minutes, then filtered to obtain acidic diatomaceous earth, and after washing away the residual hydrochloric acid in the acidic diatomaceous earth, dextran gel G50 and diatomaceous earth are mixed and ground at a mass ratio of 1:50, and then activated at 110°C for 13 minutes to obtain the additive.

[0053] Comparative Example 4

[0054] Comparative Example 4 is basically the same as Example 1, except that in step (2), the preparation method of the additive is as follows: the dextran gel G50 and diatomaceous earth are mixed and ground at a mass ratio of 1:50, and then activated at 110°C for 13 min to obtain the additive.

[0055] Comparative Example 5

[0056] Comparative Example 5 is basically the same as Example 1, except that in step (2), the preparation method of the additive is as follows: diatomaceous earth is added to a 13% hydrochloric acid solution and mixed, heated to boiling for 50 min, then filtered to obtain acidic diatomaceous earth, the residual hydrochloric acid in the acidic diatomaceous earth is washed, and then added to a 3% sodium hydroxide solution and mixed, heated to boiling for 35 min, then filtered to obtain alkaline diatomaceous earth, the residual sodium hydroxide in the alkaline diatomaceous earth is washed, and then activated at 110°C for 13 min to obtain the additive.

[0057] Comparative Example 6

[0058] Comparative Example 5 is basically the same as Example 1, except that in step (2), the auxiliary agent is dextran gel, and in step (2), the mass ratio of the auxiliary agent to Forsythia solid is 1:459.

[0059] Referring to the method provided in Wang Jianfang and Mu Xiang, Detection of Forsythoside Content in Forsythia Aqueous Extract [J]. Agricultural Development and Equipment, 2015, (03), the content and yield of forsythoside in the Forsythia leaf extracts prepared in Example 1 and Comparative Examples 1-6 were tested. The yield of forsythoside was calculated as follows: Forsythoside yield = (mass of extract * content of forsythoside in extract / mass of Forsythia leaf) * 100%. The test results are shown in Table 1.

[0060] Table 1. Effects of different adjuvants on Forsythia leaf extract.

[0061] Group Preparation method of auxiliary agent Forsythoside content (%) in the extract Forsythoside yield (%) Example 1 Acid- and alkali-treated diatomaceous earth mixed with dextran gel 67 5.05 Comparative Example 1 No additives 22 1.97 Comparative Example 2 Untreated with acid 42 3.52 Comparative Example 3 Untreated with alkali 45 3.81 Comparative Example 4 Untreated with acid or alkali 35 3.95 Comparative Example 5 Unmixed dextran gel 27 2.51 Comparative Example 6 Dextran gel additive 33 2.67

[0062] As shown in Table 1, compared with the absence of adjuvants, the use of adjuvants resulted in better separation of polysaccharides and other substances, significantly higher extraction efficiency, and significantly better selective extraction of forsythosides. Therefore, the forsythoside content and yield in the extracts were higher. Comparative Examples 5 and 6 used diatomaceous earth and dextran gel alone as adjuvants, respectively, thus only achieving a partial "auxiliary" effect, resulting in lower forsythoside content and yield in the extracts.

[0063] Compared to Example 1, Comparative Example 4 did not undergo acid and alkali treatment, resulting in poorer activity of the diatomaceous earth and a decreased binding effect with the dextran gel, which in turn affected the effectiveness of the adjuvants, ultimately leading to a decrease in the content and yield of forsythosides in the extract. Comparative Examples 2 and 3, due to the lack of complete acid and alkali treatment, showed a decrease in the content and yield of forsythosides in the extract compared to Example 1, but still achieved better extraction results than Comparative Example 4.

[0064] Example 2

[0065] Example 2 is basically the same as Example 1, except that in step (2), the mass ratio of the additive to solid A is 1:7.

[0066] Example 3

[0067] Example 3 is basically the same as Example 1, except that in step (2), the mass ratio of the additive to solid A is 1:10.

[0068] Comparative Example 7

[0069] Comparative Example 7 is basically the same as Example 1, except that in step (2), the mass ratio of the additive to solid A is 1:5.

[0070] Comparative Example 8

[0071] Comparative Example 8 is basically the same as Example 1, except that in step (2), the mass ratio of the additive to solid A is 1:12.

[0072] The content and yield of forsythoside in the forsythia leaf extracts prepared in Examples 2-3 and Comparative Examples 7-8 were tested, and the test results are shown in Table 2.

[0073] Table 2. Effects of different adjuvant dosages on Forsythia leaf extract.

[0074] Group Mass ratio of additive to solid A Forsythoside content (%) in the extract Forsythoside yield (%) Example 1 1:9 67 5.05 Example 2 1:7 65 5.02 Example 3 1:10 61 4.79 Comparative Example 7 1:5 64 4.89 Comparative Example 8 1:12 51 4.11

[0075] As shown in Table 2, when the mass ratio of the adjuvant to solid A is 1:9, the content and yield of forsythoside in the extract from which the adjuvant adsorbs and separates impurities are highest. When the amount of adjuvant is too small, impurities cannot be completely adsorbed and separated, resulting in poor extraction efficiency. Therefore, the content and yield of forsythoside in the extract of Comparative Example 8 show a significant decrease. When the amount of adjuvant is too large, there are almost no remaining impurities in the system. The excess adjuvant adsorbs some forsythoside molecules, causing a slight decrease in extraction efficiency. Therefore, the content and yield of forsythoside in the extract of Comparative Example 7 decrease slightly.

[0076] (II) Experiment on sodium hydroxide-ethanol solution

[0077] Example 4

[0078] Example 4 is basically the same as Example 1, except that in step (1), the ratio of sodium hydroxide-ethanol solution to forsythia leaf powder is 15ml:100g.

[0079] Example 5

[0080] Example 5 is basically the same as Example 1, except that in step (1), the ratio of sodium hydroxide-ethanol solution to forsythia leaf powder is 25ml:100g.

[0081] Comparative Example 9

[0082] Comparative Example 9 is basically the same as Example 1, except that in step (1), sodium hydroxide-ethanol solution is not sprayed.

[0083] Comparative Example 10

[0084] Comparative Example 10 is basically the same as Example 1, except that in step (1), the ratio of sodium hydroxide-ethanol solution to forsythia leaf powder is 5ml:100g.

[0085] The content and yield of forsythoside in the forsythia leaf extracts prepared in Examples 4-5 and Comparative Examples 9-11 were tested, and the test results are shown in Table 3.

[0086] Table 3. Effects of different amounts of sodium hydroxide-ethanol solution on the extract of Forsythia suspensa leaves.

[0087] Group The ratio of sodium hydroxide-ethanol solution to forsythia leaf powder Forsythoside content (%) in the extract Forsythoside yield (%) Example 1 20ml:100g 67 5.05 Example 4 15ml:100g 63 4.78 Example 5 25ml:100g 66 5.05 Comparative Example 9 / 57 4.01 Comparative Example 10 5ml:100g 60 4.22

[0088] Table 3 shows that the extracts sprayed with sodium hydroxide-ethanol solution all had higher forsythoside content and yield than those without. The extraction efficiency gradually increased with increasing sodium hydroxide-ethanol solution dosage, reaching its highest level when the ratio of sodium hydroxide-ethanol solution to forsythoside powder was 20 ml:100 g. However, in Example 5, further increasing the amount of sodium hydroxide-ethanol solution did not significantly change the extraction efficiency.

[0089] (II) Experimental Investigation on Steam Explosion

[0090] Example 6

[0091] Example 6 is basically the same as Example 1, except that in step (1), the blast pressure is 0.9 MPa.

[0092] Example 7

[0093] Example 7 is basically the same as Example 1, except that in step (1), the blast pressure is 2.0 MPa.

[0094] Comparative Example 11

[0095] Comparative Example 12 is basically the same as Example 1, except that steam explosion is not performed in step (1).

[0096] The content and yield of forsythoside in the forsythia leaf extracts prepared in Examples 6-7 and Comparative Example 11 were tested, and the test results are shown in Table 4.

[0097] Table 4. Effects of different steam explosion pressures on Forsythia leaf extract.

[0098] Group Steam explosion pressure (MPa) Forsythoside content (%) in the extract Forsythoside yield (%) Example 1 1.5 67 5.05 Example 6 0.9 64 4.92 Example 7 2.0 63 4.81 Comparative Example 11 / 60 4.6

[0099] Table 4 shows that the content and yield of forsythoside in the extract were highest when the steam explosion pressure was 1.5 MPa. As the steam explosion pressure increased, some large molecular structures were degraded into smaller molecules, which facilitated the dissolution and extraction of the target analyte. However, when the steam explosion pressure was too high, some large sugar molecules were degraded into polysaccharides and other substances, increasing the difficulty of subsequent separation and extraction, and slightly reducing the extraction efficiency.

[0100] Example 8

[0101] The content of Example 8 is basically the same as that of Example 1, except that the blasting time in step (1) is 110s.

[0102] Example 9

[0103] The content of Example 9 is basically the same as that of Example 1, except that the blasting time in step (1) is 200s.

[0104] The content and yield of forsythoside in the forsythia leaf extracts prepared in Examples 8-9 were tested. The test results are shown in Table 5.

[0105] Table 5. Effects of different steam explosion times on Forsythia leaf extract.

[0106] Group Steam explosion time (s) Forsythoside content (%) in the extract Forsythoside yield (%) Example 1 180 67 5.05 Example 8 110 65 4.93 Example 9 200 66 4.94

[0107] Table 5 shows that the content and yield of forsythoside in the extract were highest when the steam explosion time was 180 s. When the explosion time was too short, the overflow of the target component decreased, and the subsequent extraction effect was reduced; when the explosion time was too long, the overflow of impurities increased, which was not conducive to the extraction of forsythoside from forsythia leaves.

[0108] Example 10

[0109] A toothpaste, by mass fraction, comprises the following ingredients: 15% sorbitol, 12.5% ​​hydrated silica, 2% sodium lauryl sulfate, 4.22% polyethylene glycol 400, 8% glycerin, 1.5% CMC, 0.3% sodium saccharin, 3.8% forsythia leaf extract, 52.5% purified water, 0.05% potassium sorbate, and 0.13% sodium fluoride.

[0110] The preparation method of the forsythia leaf extract is the same as that in Example 1.

[0111] Example 11

[0112] A toothpaste with a composition that is basically the same as that in Example 10, except that it contains 2% Forsythia leaf extract and 54.3% purified water.

[0113] Example 12

[0114] A toothpaste with a composition that is basically the same as that in Example 10, except that it contains 5% Forsythia leaf extract and 51.3% purified water.

[0115] Performance testing:

[0116] Fifty patients with oral ulcers were selected, with similar ages and severity of ulcers. They were randomly divided into four groups: Control Group 1, Experimental Group 1, Experimental Group 2, and Experimental Group 3. Control Group 1 used regular toothpaste for 5 consecutive days; Experimental Group 1 used toothpaste prepared in Example 10 for 5 consecutive days; Experimental Group 2 used toothpaste prepared in Example 11 for 5 consecutive days; and Experimental Group 3 used toothpaste prepared in Example 12 for 5 consecutive days. The effectiveness of toothpaste treatment was recorded on the 3rd and 5th days of continuous use. The evaluation criteria were as follows:

[0117] Cure: The erosion has completely healed, the white or gray lines and congestion have subsided, and the subjective symptoms have disappeared;

[0118] Significant effect: The erosion surface heals without congestion, and more than 2 / 3 of the white or gray lines disappear, with symptoms significantly reduced;

[0119] Improvement: Less than 2 / 3 of the white or gray lines in the mouth have disappeared, and the symptoms have been partially relieved. The results are recorded in Table 6.

[0120] Table 6. Effects of different toothpastes on patients with oral ulcers.

[0121]

[0122] As shown in Table 6, compared with ordinary toothpaste, the toothpaste prepared according to this application can effectively reduce the healing time of oral ulcers; moreover, the effect is more obvious with the increase of the amount of Forsythia suspensa leaf extract. According to the characteristics of toothpaste products, the maximum amount of Forsythia suspensa extract in toothpaste is 5%. Therefore, when the Forsythia suspensa extract in toothpaste is 5%, the toothpaste has the best effect on oral ulcers.

[0123] The foregoing has described preferred embodiments of the present invention. However, it should be understood that the invention is not limited to the content disclosed herein. Any non-substantial improvements made using the inventive concept and technical solution, or any application of the inventive concept and technical solution to other situations, are within the protection scope of the present invention.

Claims

1. A method for preparing Forsythia suspensa leaf extract, characterized by, The method comprises the following steps: (1) treating fortemptation, drying and crushing of Forsythia suspensa leaves to obtain Forsythia suspensa leaf powder; spraying sodium hydroxide-ethanol solution on the Forsythia suspensa leaf powder, then sealing and standing for 12-24 hours, and then sequentially performing drying and steam explosion to obtain solid A; (2) refluxing extraction of the solid A with ethanol solution, then performing solid-liquid separation to obtain filtrate A; concentrating the filtrate A to obtain concentrated solution A, adding anhydrous ethanol and an additive to the concentrated solution A, stirring at 50-60 DEG C for 20-30 minutes, then standing, and then performing solid-liquid separation to obtain filtrate B; adding water to the paste-like filtrate B, mixing, and then concentrating to obtain concentrated solution B; (3) standing the concentrated solution B at room temperature for 5-10 hours, then performing solid-liquid separation, collecting the solid, and drying to obtain Forsythia suspensa leaf extract; The additive is prepared by the following method: adding diatomite to an acidic solution, mixing, heating to boiling, and then filtering to obtain acidic diatomite; washing the acidic diatomite, adding to an alkaline solution, mixing, heating to boiling, and then filtering to obtain alkaline diatomite; and mixing, grinding and activating the alkaline diatomite with dextran gel to obtain the additive; The mass ratio of the dextran gel to the diatomite is 1:(30-60); the dextran gel is any one of G10, G50 and G100; In step (1), the use amount ratio of the Forsythia suspensa leaf powder to the sodium hydroxide-ethanol solution is 100 g:(15-25) ml; the sodium hydroxide content in the sodium hydroxide-ethanol solution is 0.2-0.5 g / L; and the steam explosion pressure is 0.9-2.0 MPa and the time is 110-200 seconds; In step (2), the material-liquid ratio of the refluxing extraction is 1 g:(7-11) ml and the extraction time is 1-3 hours; the volume ratio of the concentrated solution A to anhydrous ethanol is 1:(2-3) and the mass ratio of the additive to the solid A is 1:(7-10). The acidic solution is a hydrochloric acid solution with a mass fraction of 10-15%; and the alkaline solution is a sodium hydroxide solution with a mass fraction of 2-5%.

2. The process for the preparation of forsythia leaf extract as claimed in claim 1, wherein, Prepared by the preparation method of claim 1 or 2.

3. Forsythia suspensa leaf extract, characterized in that, 4. The Forsythia suspensa leaf extract of claim 3 is used in toothpaste. The toothpaste comprises the Forsythia suspensa leaf extract of claim 3.

5. A toothpaste, characterized by The toothpaste comprises the Forsythia suspensa leaf extract of claim 3.

6. The toothpaste according to claim 5, wherein The toothpaste comprises the Forsythia suspensa leaf extract of claim 3.

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