Traditional Chinese medicine toothpaste for preventing and treating gingivitis and preparation method thereof

Abstract

The invention discloses traditional Chinese medicine toothpaste, and particularly relates to traditional Chinese medicine toothpaste for preventing and treating gingivitis and a preparation method of the traditional Chinese medicine toothpaste. The traditional Chinese medicine toothpaste is prepared from the following components in percentage by mass: 0.05 to 5 percent of rhizoma bletillae polysaccharide, 0.1 to 10 percent of inclusion compound obtained by inclusion of piper cubeba volatile oil with beta-cyclodextrin, 5 to 30 percent of silicon dioxide, 30 to 70 percent of humectant, 0.05 to 0.5 percent of aromatic, 0.05 to 5 percent of foaming agent, 0.1 to 1 percent of sweetening agent, 0.0001 to 0.5 percent of coloring agent, 0.1 percent of preservative and the balance of deionized water. The rhizoma bletillae polysaccharide and the piper cubeba volatile oil beta-cyclodextrin inclusion compound are combined for preventing and treating gingivitis, can synergistically resist bacteria and inflammation, improve gingival microcirculation and achieve the effects of diminishing inflammation, relieving pain and stopping bleeding, on the basis, healing of damaged gingiva is accelerated, the recovery time of gingivitis of a patient is shortened, and the pain of the patient is relieved; the effects of a thickening agent and essence in the auxiliary materials can be reduced or replaced, the effects of thickening and flavoring are achieved by utilizing the characteristics of the rhizoma bletillae polysaccharide and the piper cubeba volatile oil, and the medicines and the auxiliary materials are combined.

Description

Technical Field

[0001] The present invention relates to the technical field of toothpaste, and particularly to a traditional Chinese medicine toothpaste for preventing and treating gingivitis and a preparation method thereof. Background Art

[0002] Gingival inflammation is a chronic oral disease characterized by inflammation of the gingival tissue. The symptoms of gingivitis generally include gingival redness, gingival bleeding, gingival pain, tooth loosening, bad breath, etc. The pathogenesis of gingivitis is divided into initial, early, and established stages. When chronic gingivitis only affects the gingiva, the condition can be reversed using appropriate treatment methods. However, if chronic gingivitis is not effectively controlled, it may further develop into periodontitis and even lead to tooth loss, seriously affecting the quality of life of patients.

[0003] Dental plaque biofilm is considered to be the precursor of gingivitis. Research shows that removing microbial plaque can eliminate gingival inflammation, and stopping plaque control can lead to the recurrence of gingival inflammation. Therefore, continuous removal of plaque by brushing is considered to be the most effective means of preventing and controlling gingivitis. However, with the existing brushing methods and the toothpaste used, most people find it difficult to maintain a plaque control level commensurate with periodontal health. Therefore, supplementing additional active therapeutic ingredients in toothpaste is considered to be a direct and effective method for controlling gingival inflammation.

[0004] Bletilla striata is the dried tuber of the orchid plant Bletilla striata. Its main functions are to astringe sores and stop bleeding, disperse swelling and promote granulation. Its extract, Bletilla striata polysaccharide, has strong antibacterial effects, is closely related to the inhibition of dental plaque and dental caries, and also has strong inhibitory effects on Streptococcus mutans. At the same time, Bletilla striata polysaccharide also has the effects of promoting the growth of granulation tissue, protecting the wound surface, and accelerating wound healing. Chinese Patent CN109276475B discloses a traditional Chinese medicine toothpaste containing Bletilla striata polysaccharide, which is composed of the following components in weight percentage: Bletilla striata polysaccharide 1 - 5%, emodin 0.1 - 0.5%, glycerol 5 - 20%, sorbitol solution 30 - 60%, saccharin sodium 0.1 - 0.5%, carboxymethyl cellulose sodium 1 - 5%, abrasive silica 10 - 25%, thickening silica 5 - 10%, sodium lauryl sulfate 1 - 5%, menthol 0.5 - 1%, sodium benzoate 0.1 - 0.5%, and the balance is deionized water. The emodin and Bletilla striata polysaccharide in the traditional Chinese medicine toothpaste have a synergistic effect, which can comprehensively solve oral problems such as gingival inflammation and the resulting gingival bleeding and oral ulcers, achieving both symptomatic and root cause treatment. However, the above traditional Chinese medicine toothpaste also has the following disadvantages:

[0005] (1) The curative effect of traditional Chinese medicine toothpaste for preventing and treating common oral diseases such as periodontitis, gingivitis, gingival bleeding, and gingival swelling and pain is not high enough;

[0006] (2) The quality of traditional Chinese medicine toothpaste is not good. As the storage time prolongs, the effective substances volatilize, resulting in a worse curative effect;

[0007] (3) The thickener content in traditional Chinese medicine toothpaste is relatively high. Summary of the Invention

[0008] The purpose of the present invention is to provide a traditional Chinese medicine toothpaste for preventing and treating gingivitis and its preparation method, so as to solve the problems of poor efficacy, poor stability and excessive addition of auxiliaries in the above-mentioned traditional Chinese medicine toothpaste.

[0009] To achieve the above purpose, the first aspect of the present invention provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis, and the traditional Chinese medicine toothpaste comprises the following components according to mass fraction:

[0010] Bletilla striata polysaccharide 0.05 - 5%, β-cyclodextrin inclusion complex of Litsea cubeba volatile oil 0.1 - 10%, silicon dioxide 5 - 30%, humectant 30 - 70%, flavoring agent 0.05 - 0.5%, foaming agent 0.05 - 5%, sweetening agent 0.1 - 1%, coloring agent 0.0001 - 0.5%, preservative 0.1% and the balance deionized water.

[0011] Preferably, the traditional Chinese medicine toothpaste comprises the following components according to mass fraction:

[0012] Bletilla striata polysaccharide 0.3 - 1.3%, β-cyclodextrin inclusion complex of Litsea cubeba volatile oil 0.7 - 1.7%, silicon dioxide 10 - 20%, humectant 45 - 55%, flavoring agent 0.2 - 0.3%, foaming agent 1.5 - 2.5%, sweetening agent 0.1 - 0.3%, coloring agent 0.0005 - 0.0015%, preservative 0.1% and the balance deionized water.

[0013] Preferably, the silicon dioxide comprises at least one of thickening type silicon dioxide and friction type silicon dioxide.

[0014] Preferably, the purity of Bletilla striata polysaccharide is 10% - 90%; the humectant is selected from at least one of sorbitol, polyethylene glycol, glycerol and propylene glycol; the flavoring agent is selected from at least one of menthol, peppermint oil and eucalyptus oil; the foaming agent is selected from at least one of sodium dodecyl sulfate, sodium lauroyl sarcosinate and cocamidopropyl betaine; the sweetening agent is selected from at least one of sodium saccharin, trichlorogalactose, stevioside and xylitol; the coloring agent is selected from at least one of sunset yellow, lemon yellow, gardenia yellow and safflower yellow; the preservative is selected from at least one of parabens, benzoic acid and sorbic acid.

[0015] The second aspect of the present invention provides a preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis, comprising the following steps:

[0016] S1: Inclusion of Litsea cubeba volatile oil with β-cyclodextrin to obtain β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, and reserve it;

[0017] S2: Add deionized water to the Bletilla striata polysaccharide, heat and stir to obtain an aqueous solution of Bletilla striata polysaccharide;

[0018] S3: Dissolve the sweetener, flavoring agent and preservative in water, and mix with the humectant to obtain a mixed solution for standby;

[0019] S4: Mix the β - cyclodextrin inclusion complex of Litsea cubeba volatile oil, silicon dioxide and foaming agent evenly to obtain a mixture for standby;

[0020] S5: Add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture and the coloring agent to the paste - making tank in sequence, stir evenly, evacuate with a paste - making machine, and fill to obtain the traditional Chinese medicine toothpaste.

[0021] Preferably, in step S1, the specific preparation process of the β - cyclodextrin inclusion complex of Litsea cubeba volatile oil is as follows:

[0022] S11: Extract the Litsea cubeba volatile oil from the Litsea cubeba raw material for standby;

[0023] S12: Dissolve the Litsea cubeba volatile oil in 95% ethanol to obtain a Litsea cubeba ethanol solution for standby;

[0024] S13: Add deionized water to β - cyclodextrin, mix evenly to obtain a β - cyclodextrin solution for standby;

[0025] S14: Add the Litsea cubeba ethanol solution to the β - cyclodextrin solution, perform inclusion, and after standing, filtering and drying, obtain the β - cyclodextrin inclusion complex of Litsea cubeba volatile oil.

[0026] Preferably, in step S11, the method for extracting Litsea cubeba volatile oil is one of steam distillation method, supercritical fluid extraction method or pressing method. After extraction, it is dehydrated with anhydrous sodium sulfate or silica gel to obtain Litsea cubeba volatile oil.

[0027] Preferably, in step S12, the mass ratio of Litsea cubeba volatile oil to 95% ethanol is 1:0.1 - 2;

[0028] Preferably, in step S13, add 10 - 40 times deionized water to β - cyclodextrin, heat to 30 - 70°C, and after β - cyclodextrin is completely dissolved, cool to 20 - 60°C to obtain a β - cyclodextrin solution.

[0029] Preferably, in step S14, the inclusion method of the β - cyclodextrin inclusion complex of Litsea cubeba volatile oil is one of saturated aqueous solution method, ultrasonic method, grinding method, freeze - drying method or spray - drying method.

[0030] Preferably, in step S14, the inclusion time is 1 - 5 h; the standing temperature is 4 - 8°C, the standing time is 10 - 30 h; the drying temperature is 20 - 60°C, and the drying time is 1 - 10 h.

[0031] Preferably, in step S2, 7-13 times deionized water is added to the Bletilla striata polysaccharide, heated to 30-70 °C, and stirred for 1-10 h to obtain an aqueous solution of Bletilla striata polysaccharide.

[0032] In step S5, the stirring speed is 20-180 r / min, and the stirring time is 20-80 min.

[0033] Therefore, the present invention adopts the above-mentioned traditional Chinese medicine toothpaste for preventing and treating gingivitis and its preparation method, and has the following beneficial effects:

[0034] (1) In the present invention, the combination of Bletilla striata polysaccharide and the essential oil of Litsea cubeba can synergistically antibacterial and anti-inflammatory, improve the microcirculation of the gums, achieve the effects of anti-inflammatory, analgesic and hemostatic, and on this basis, accelerate the healing of damaged gums, shorten the recovery time of patients with gingivitis, reduce the pain of patients, and make the gums and teeth healthier.

[0035] (2) The combined application of Bletilla striata polysaccharide and the essential oil of Litsea cubeba in the present invention can also reduce or replace the functions of thickeners and flavors in the excipients, and utilize the self-characteristics of Bletilla striata polysaccharide and the essential oil of Litsea cubeba to play the roles of thickening and flavoring, integrating medicine and excipient.

[0036] Next, through examples, the technical solutions of the present invention will be further described in detail. Specific Embodiments

[0037] The present invention will be further described below. It should be noted that this embodiment is based on the present technical solution, and gives detailed implementation manners and specific operation processes, but the present invention is not limited to this embodiment.

[0038] Example 1

[0039] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis, and the traditional Chinese medicine toothpaste includes the following components:

[0040] 1 g of Bletilla striata polysaccharide, 5 g of β-cyclodextrin inclusion complex of the essential oil of Litsea cubeba, 28 g of thickening silica, 42 g of abrasive silica, 300 g of sorbitol, 1 g of menthol, 12 g of sodium lauryl sulfate, 1.2 g of saccharin sodium, 0.002 g of tartrazine, 1 g of nipagin ester, and deionized water is added to make up to 1000 g.

[0041] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0042] S1. The preparation method of the β-cyclodextrin inclusion complex of the essential oil of Litsea cubeba is as follows:

[0043] The volatile oil of Litsea cubeba is included with β-cyclodextrin to obtain the inclusion compound of the volatile oil of Litsea cubeba-β-cyclodextrin for standby; specifically:

[0044] S11. Place the Litsea cubeba medicinal materials in a press, add a small amount of deionized water, squeeze out the volatile oil in the medicinal materials through mechanical extrusion, collect the squeezed oil-water mixture, centrifuge, take the upper layer of oil liquid, filter, and then dehydrate with anhydrous sodium sulfate to obtain the volatile oil of Litsea cubeba;

[0045] S12: Dissolve the volatile oil of Litsea cubeba in 95% ethanol according to a ratio to obtain a Litsea cubeba ethanol solution for use;

[0046] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄挥乙醇溶液 : m β-环糊精 = 1:0.1) to 10 times the amount of deionized water, heat to 30 °C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 20 °C to obtain a β-cyclodextrin solution for use.

[0047] S14. Slowly drop the Litsea cubeba ethanol solution into the β-cyclodextrin solution under stirring, include for 1 h, place at 4 °C for 10 h, filter while it is cold, and dry the precipitate at normal pressure at 20 °C for 1 hour to obtain the inclusion compound of the volatile oil of Litsea cubeba-β-cyclodextrin.

[0048] The above materials are made into toothpaste according to the following steps:

[0049] S2. Add the polysaccharide of Bletilla striata to 7 times the amount of deionized water, heat to 30 °C, and stir for 1 h to obtain an aqueous solution of the polysaccharide of Bletilla striata for use.

[0050] S3. Dissolve sodium saccharin, menthol, and nipagin ester in water and mix with sorbitol to obtain a mixed solution for use.

[0051] S4. Mix the inclusion compound of the volatile oil of Litsea cubeba-β-cyclodextrin, thickening silica, abrasive silica, and sodium lauryl sulfate evenly to obtain a mixture for use.

[0052] S5. Add the aqueous solution of the polysaccharide of Bletilla striata, the mixed solution, the mixture, and lemon yellow to the paste-making tank in sequence, stir at a speed of 20 r / min for 20 min, evacuate the paste-making machine, and fill to obtain the toothpaste.

[0053] Example 2

[0054] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0055] 2 g of Bletilla striata polysaccharide, 6 g of β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, 25 g of thickening silica, 45 g of friction silica, 350 g of glycerol, 1.2 g of peppermint oil, 14 g of sodium lauroyl sarcosinate, 1.4 g of xylitol, 0.004 g of sunset yellow, 1 g of benzoic acid, and deionized water was added to make up to 1000 g.

[0056] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0057] S1. The preparation method of the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil is as follows:

[0058] The Litsea cubeba volatile oil was included with β-cyclodextrin to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil for standby; specifically:

[0059] S11. The Litsea cubeba medicinal materials were placed in a supercritical CO2 extraction kettle, the CO2 was cooled to -4 °C, and it was pumped into the system at a flow rate of 1.5 ml / min for extraction. The extraction temperature was 45 °C, the extraction pressure was 25 MPa. The extraction product was collected, centrifuged, and the upper layer of oil was taken. After dehydration with silica gel, Litsea cubeba volatile oil was obtained.

[0060] S12. The Litsea cubeba volatile oil was dissolved in 95% ethanol in proportion to obtain a Litsea cubeba ethanol solution for standby.

[0061] S13. A certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:0.2) was added to 12 times the amount of deionized water and heated to 30 °C. After the β-cyclodextrin was completely dissolved, the temperature was lowered to 20 °C to obtain a β-cyclodextrin solution for standby.

[0062] S14. The Litsea cubeba ethanol solution and the β-cyclodextrin solution were mixed in a mortar, ground in a water bath at 50 °C for 2 h, allowed to stand, and filtered by suction. The precipitate was vacuum dried at 30 °C for 2 hours to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil.

[0063] The above materials were made into toothpaste according to the following steps:

[0064] S2. The Bletilla striata polysaccharide was added to 8 times the amount of deionized water and heated to 40 °C, stirred for 2 h to obtain a Bletilla striata polysaccharide aqueous solution for standby.

[0065] S3. The xylitol, peppermint oil, and benzoic acid were dissolved in water and mixed with glycerol to obtain a mixed solution for standby;

[0066] S4. The β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, thickening silica, friction silica, and sodium lauroyl sarcosinate were mixed evenly to obtain a mixture for standby;

[0067] S5. Sequentially add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture, and sunset yellow into the paste-making tank, stir at a speed of 30 r / min for 30 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0068] Example 3

[0069] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0070] 4 g of Bletilla striata polysaccharide, 8 g of β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, 44 g of thickening silica, 66 g of friction-type silica, 400 g of polyethylene glycol, 2 g of eucalyptus oil, 16 g of cocamidopropyl betaine, 1.6 g of trichlorogalactose, 0.006 g of gardenia yellow, 1 g of sorbic acid, and deionized water is added to make up to 1000 g.

[0071] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0072] S1. The preparation method of the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil is as follows:

[0073] Use β-cyclodextrin to include Litsea cubeba volatile oil to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, and set it aside; specifically:

[0074] S11. Place the Litsea cubeba medicinal materials in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper layer of oil liquid, and then dehydrate it with anhydrous sodium sulfate to obtain Litsea cubeba volatile oil.

[0075] S12. Dissolve the Litsea cubeba volatile oil in 95% ethanol according to the proportion to obtain the Litsea cubeba ethanol solution for use.

[0076] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:0.4) to 14 times the amount of deionized water, heat to 30 °C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 20 °C to obtain the β-cyclodextrin solution for use.

[0077] S14. Mix the Litsea cubeba ethanol solution and the β-cyclodextrin solution in a mortar, grind on a 40 °C water bath for 3 h, let it stand, filter by suction, and vacuum dry the precipitate at 40 °C for 1 hour to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil.

[0078] Make the above materials into toothpaste according to the following steps:

[0079] S2. Add the Bletilla striata polysaccharide into 9 times the amount of deionized water, heat to 50 °C, and stir for 3 h to obtain an aqueous solution of Bletilla striata polysaccharide for later use.

[0080] S3. Dissolve trichlorogalactose, eucalyptus oil, and sorbic acid in water, and mix with polyethylene glycol to obtain a mixed solution for later use.

[0081] S4. Mix the β-cyclodextrin inclusion complex of Piper cubeba volatile oil, thickening silica, friction silica, and cocamidopropyl betaine evenly to obtain a mixture for later use.

[0082] S5. Add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture, and gardenia yellow into the paste-making tank in sequence, stir at a speed of 40 r / min for 40 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0083] Example 4

[0084] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0085] 6 g of Bletilla striata polysaccharide, 10 g of β-cyclodextrin inclusion complex of Piper cubeba volatile oil, 43 g of thickening silica, 77 g of friction silica, 450 g of propylene glycol, 1.2 g of menthol, 1.2 g of eucalyptus oil, 9 g of sodium dodecyl sulfate, 9 g of sodium lauroyl sarcosinate, 1.8 g of stevioside, 0.008 g of carthamin yellow, 1 g of sorbic acid, and make up to 1000 g with deionized water.

[0086] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0087] S1. The preparation method of the β-cyclodextrin inclusion complex of Piper cubeba volatile oil is as follows:

[0088] Carry out inclusion of Piper cubeba volatile oil with β-cyclodextrin to obtain the β-cyclodextrin inclusion complex of Piper cubeba volatile oil for standby; specifically:

[0089] S11. Place the Piper cubeba medicinal materials in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper layer of oil, and then dehydrate it with anhydrous sodium sulfate to obtain Piper cubeba volatile oil.

[0090] S12. Dissolve the Piper cubeba volatile oil in 95% ethanol in proportion to obtain a Piper cubeba ethanol solution for later use.

[0091] S13. Take a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精(ratio = 1:0.6) was added to 16 times the amount of deionized water and heated to 30 °C. After the β-cyclodextrin was completely dissolved, the temperature was lowered to 20 °C to obtain a β-cyclodextrin solution for later use.

[0092] S14. Mix the ethanol solution of Litsea cubeba and the β-cyclodextrin solution in a mortar, grind them in a water bath at 60 °C for 1 h, let it stand, filter by suction, and vacuum dry the precipitate at 60 °C for 3 hours to obtain the Litsea cubeba volatile oil β-cyclodextrin inclusion compound.

[0093] The above materials were made into toothpaste according to the following steps:

[0094] S2. Add the polysaccharide of Bletilla striata to 11 times the amount of deionized water, heat to 55 °C, and stir for 4 h to obtain an aqueous solution of the polysaccharide of Bletilla striata for later use.

[0095] S3. Dissolve stevioside, menthol, eucalyptus oil, and sorbic acid in water and mix with propylene glycol to obtain a mixed solution for later use.

[0096] S4. Mix the Litsea cubeba volatile oil β-cyclodextrin inclusion compound, thickening silica, abrasive silica, sodium lauryl sulfate, and sodium lauroyl sarcosinate evenly to obtain a mixture for later use.

[0097] S5. Add the aqueous solution of the polysaccharide of Bletilla striata, the mixed solution, the mixture, and safflower yellow to the paste-making tank in sequence, stir at a speed of 60 r / min for 45 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0098] Example 5

[0099] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0100] 8 g of polysaccharide of Bletilla striata, 12 g of Litsea cubeba volatile oil β-cyclodextrin inclusion compound, 50 g of thickening silica, 100 g of abrasive silica, 480 g of sorbitol, 3 g of menthol, 20 g of sodium lauryl sulfate, 2 g of saccharin sodium, 0.01 g of lemon yellow, 0.1% of sorbic acid, and deionized water was added to make up to 1000 g.

[0101] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0102] S1. The preparation method of the Litsea cubeba volatile oil β-cyclodextrin inclusion compound is as follows:

[0103] The Litsea cubeba volatile oil was included by β-cyclodextrin to obtain the Litsea cubeba volatile oil β-cyclodextrin inclusion compound for standby; specifically:

[0104] S11. Place the cubeb fruits in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper layer of oil, and then dehydrate it with silica gel to obtain cubeb volatile oil.

[0105] S12. Dissolve the cubeb volatile oil in 95% ethanol in proportion to obtain a cubeb ethanol solution for later use.

[0106] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 :m β-环糊精 = 1:0.5) to 25 times the amount of deionized water, heat to 50 °C, and after β-cyclodextrin is completely dissolved, lower the temperature to 40 °C to obtain a β-cyclodextrin solution for later use.

[0107] S14. Slowly drip the cubeb ethanol solution into the β-cyclodextrin solution under stirring, perform inclusion for 3 h, and place it at 4 °C for 24 h. Filter while it is cold, and dry the precipitate at normal pressure at 40 °C for 3 hours to obtain a cubeb volatile oil β-cyclodextrin inclusion complex.

[0108] The above materials are made into toothpaste according to the following steps:

[0109] S2. Add the bletilla striata polysaccharide to 10 times the amount of deionized water, heat to 50 °C, and stir for 5 h to obtain a bletilla striata polysaccharide aqueous solution for later use.

[0110] S3. Dissolve sodium saccharin, menthol, and sorbic acid in water and mix with sorbitol to obtain a mixed solution for later use.

[0111] S4. Mix the cubeb volatile oil β-cyclodextrin inclusion complex, thickening silica, abrasive silica, and sodium lauryl sulfate evenly to obtain a mixture for later use.

[0112] S5. Add the bletilla striata polysaccharide aqueous solution, the mixed solution, the mixture, and tartrazine to the paste-making tank in sequence, stir at a speed of 100 r / min for 50 min, evacuate the paste-making machine, and fill to obtain the toothpaste.

[0113] Example 6

[0114] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0115] 10 g of Bletilla striata polysaccharide, 14 g of β-cyclodextrin inclusion compound of Litsea cubeba volatile oil, 43 g of thickening silica, 127 g of friction silica, 150 g of propylene glycol, 150 g of glycerin, 200 g of sorbitol, 2 g of menthol, 1 g of peppermint oil, 1 g of eucalyptus oil, 20 g of sodium lauroyl sarcosinate, 10 g of coconut oil amide propyl betaine, 1 g of trichlorogalactose, 1 g of sodium saccharin, 1 g of xylitol, 0.01 g of tartrazine, 0.01 g of sunset yellow, 1 g of nipagin ester, and deionized water is added to make up to 1000 g.

[0116] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis comprises the following steps:

[0117] S1. The preparation method of the β-cyclodextrin inclusion compound of Litsea cubeba volatile oil is as follows:

[0118] The Litsea cubeba volatile oil is included by β-cyclodextrin to obtain the β-cyclodextrin inclusion compound of Litsea cubeba volatile oil for standby.

[0119] S11. Place the Litsea cubeba medicinal materials in a supercritical CO2 extraction kettle, cool CO2 to -4°C, pump it into the system at a flow rate of 1.5 ml / min for extraction, the extraction temperature is 45°C, the extraction pressure is 25 MPa, collect the extraction product, centrifuge, take the upper layer of oil liquid, and then dehydrate it with anhydrous sodium sulfate to obtain Litsea cubeba volatile oil.

[0120] S12. Dissolve the Litsea cubeba volatile oil in 95% ethanol in proportion to obtain a Litsea cubeba ethanol solution for standby.

[0121] S2. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:0.7) to 20 times the amount of deionized water, heat it to 70°C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 60°C to obtain a β-cyclodextrin solution for standby.

[0122] S3. Add the Litsea cubeba ethanol solution to the β-cyclodextrin solution, perform inclusion for 30 min in an ultrasonic cleaner (power 250 W, frequency 40 KHz), let it stand, filter by suction, and dry the precipitate at 60°C under normal pressure for 6 hours to obtain the β-cyclodextrin inclusion compound of Litsea cubeba volatile oil.

[0123] The above materials are made into toothpaste according to the following steps:

[0124] S2. Add the Bletilla striata polysaccharide to 13 times the amount of deionized water, heat it to 60°C, and stir for 6 h to obtain a Bletilla striata polysaccharide aqueous solution for standby.

[0125] S3. Dissolve trichlorogalactose, xylitol, sodium saccharin, menthol, peppermint oil, eucalyptus oil, and sorbic acid in water, and mix them with propylene glycol, glycerin, and sorbitol to obtain a mixed solution for standby.

[0126] S4. Mix the β-cyclodextrin inclusion complex of cubeb essential oil, thickening silica, friction silica, cocamidopropyl betaine, and sodium lauroyl sarcosinate evenly to obtain a mixture for later use.

[0127] S5. Add the aqueous solution of bletilla striata polysaccharide, the mixed solution, the mixture, tartrazine, and sunset yellow to the paste-making tank in sequence, stir at a speed of 80 r / min for 60 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0128] Example 7

[0129] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste comprises the following components:

[0130] 12 g of bletilla striata polysaccharide, 16 g of β-cyclodextrin inclusion complex of cubeb essential oil, 55 g of thickening silica, 135 g of friction silica, 150 g of glycerol, 200 g of polyethylene glycol, 200 g of propylene glycol, 2.5 g of peppermint oil, 2.5 g of eucalyptus oil, 20 g of sodium dodecyl sulfate, 20 g of cocamidopropyl betaine, 2 g of stevioside, 2 g of xylitol, 0.01 g of tartrazine, 0.02 g of gardenia yellow, 1 g of benzoic acid, and deionized water is added to make up to 1000 g.

[0131] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis comprises the following steps:

[0132] S1. The preparation method of the β-cyclodextrin inclusion complex of cubeb essential oil is as follows:

[0133] Use β-cyclodextrin to include cubeb essential oil to obtain the β-cyclodextrin inclusion complex of cubeb essential oil for standby; specifically:

[0134] S11. Place the cubeb medicinal materials in a press, add a small amount of deionized water, squeeze out the essential oil in the medicinal materials by mechanical extrusion, collect the squeezed oil-water mixture, centrifuge, take the upper-layer oil liquid, filter, and then dehydrate with silica gel to obtain cubeb essential oil.

[0135] S12. Dissolve the cubeb essential oil in 95% ethanol in proportion to obtain a cubeb ethanol solution for later use.

[0136] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:0.8) to 30 times the amount of deionized water, heat to 65 °C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 55 °C to obtain a β-cyclodextrin solution for later use.

[0137] S14. Add the ethanol solution of Litsea cubeba oil into the β-cyclodextrin solution, and perform inclusion for 20 min in an ultrasonic cleaner (power 300 W, frequency 50 KHz), then let it stand, filter by suction, and dry the precipitate under normal pressure at 55 °C for 8 hours to obtain the Litsea cubeba oil β-cyclodextrin inclusion compound.

[0138] The above materials are made into toothpaste according to the following steps:

[0139] S2. Add Bletilla striata polysaccharide into 12 times the amount of deionized water, heat to 70 °C, and stir for 8 h to obtain the aqueous solution of Bletilla striata polysaccharide for later use.

[0140] S3. Dissolve stevioside, xylitol, peppermint oil, eucalyptus oil, and benzoic acid in water, and mix with glycerol, polyethylene glycol, and propylene glycol to obtain a mixed solution for later use.

[0141] S4. Mix the Litsea cubeba oil β-cyclodextrin inclusion compound, thickening silica, abrasive silica, cocamidopropyl betaine, and sodium lauryl sulfate evenly to obtain a mixture for later use.

[0142] S5. Add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture, sunset yellow, and gardenia yellow into the paste-making tank in sequence, stir at a speed of 80 r / min for 60 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0143] Example 8

[0144] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0145] 14 g of Bletilla striata polysaccharide, 18 g of Litsea cubeba oil β-cyclodextrin inclusion compound, 70 g of thickening silica, 140 g of abrasive silica, 400 g of sorbitol, 200 g of glycerol, 5.5 g of menthol, 50 g of sodium lauryl sulfate, 2.5 g of saccharin sodium, 2 g of stevioside, 0.01 g of carthamin yellow, 0.01 g of gardenia yellow, 0.02 g of sunset yellow, 0.1% of sorbic acid, and make up to 1000 g with deionized water.

[0146] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0147] S1. The preparation method of the Litsea cubeba oil β-cyclodextrin inclusion compound is as follows:

[0148] Perform inclusion of Litsea cubeba oil with β-cyclodextrin to obtain the Litsea cubeba oil β-cyclodextrin inclusion compound for standby; specifically:

[0149] S11. Place the cubeb fruits in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper layer of oil, and then dehydrate it with silica gel to obtain cubeb volatile oil.

[0150] S12. Dissolve the cubeb volatile oil in 95% ethanol in proportion to obtain a cubeb ethanol solution for later use.

[0151] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:1) to 40 times the amount of deionized water, heat to 70 °C, and after β-cyclodextrin is completely dissolved, lower the temperature to 60 °C to obtain a β-cyclodextrin solution for later use.

[0152] S14. Add the cubeb ethanol solution to the β-cyclodextrin solution, and perform inclusion for 35 min in an ultrasonic cleaner (power 200 W, frequency 30 KHz), let it stand, filter by suction, and vacuum dry the precipitate at 60 °C for 10 hours to obtain a cubeb volatile oil β-cyclodextrin inclusion complex.

[0153] The above materials are made into toothpaste according to the following steps:

[0154] S2. Add bletilla striata polysaccharide to 13 times the amount of deionized water, heat to 55 °C, and stir for 10 h to obtain a bletilla striata polysaccharide aqueous solution for later use.

[0155] S3. Dissolve stevioside, saccharin sodium, menthol, and sorbic acid in water, and mix them with glycerol and sorbitol to obtain a mixed solution for later use.

[0156] S4. Mix the cubeb volatile oil β-cyclodextrin inclusion complex, thickening silica, abrasive silica, and sodium lauryl sulfate evenly to obtain a mixture for later use.

[0157] S5. Add the bletilla striata polysaccharide aqueous solution, the mixed solution, the mixture, and sunset yellow, safflower yellow, and gardenia yellow to the paste-making tank in sequence, stir at a speed of 120 r / min for 80 min, evacuate the paste-making machine, and fill to obtain toothpaste.

[0158] Example 9

[0159] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0160] 0.5 g of Bletilla striata polysaccharide, 1 g of β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, 50 g of thickening silica, 100 g of friction silica, 200 g of glycerol, 200 g of polyethylene glycol, 300 g of sorbitol, 5 g of menthol, 50 g of sodium lauryl sulfate, 10 g of xylitol, 3 g of tartrazine, 2 g of safflower yellow, 1 g of nipagin ester, and deionized water is added to make up to 1000 g.

[0161] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis comprises the following steps:

[0162] S1. The preparation method of the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil is as follows:

[0163] The Litsea cubeba volatile oil is included with β-cyclodextrin to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil for standby; specifically:

[0164] S11. Place the Litsea cubeba medicinal materials in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper layer of oil liquid, and then dehydrate with silica gel to obtain Litsea cubeba volatile oil.

[0165] S12. Dissolve the Litsea cubeba volatile oil in 95% ethanol in proportion to obtain a Litsea cubeba ethanol solution for standby.

[0166] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:0.6) to 25 times the amount of deionized water, heat to 45 °C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 35 °C to obtain a β-cyclodextrin solution for standby.

[0167] S14. Add the Litsea cubeba ethanol solution to the β-cyclodextrin solution, mix evenly, freeze in a -20 °C refrigerator for 12 h, take out, and place in a freeze dryer for freeze drying at 50 °C for 24 h to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil.

[0168] The above materials are made into toothpaste according to the following steps:

[0169] S2. Add the Bletilla striata polysaccharide to 10 times the amount of deionized water, heat to 60 °C, and stir for 4 h to obtain a Bletilla striata polysaccharide aqueous solution for standby.

[0170] S3. Dissolve xylitol, menthol, and nipagin ester in water and mix with sorbitol to obtain a mixed solution for standby.

[0171] S4. Mix the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, thickening silica, friction silica, and sodium lauryl sulfate evenly to obtain a mixture for standby.

[0172] S5. Add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture, tartrazine, and safflower yellow into the paste-making tank in sequence, stir at a speed of 160 r / min for 75 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0173] Example 10

[0174] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste comprises the following components:

[0175] 50 g of Bletilla striata polysaccharide, 100 g of β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, 100 g of thickening silica, 200 g of friction silica, 100 g of polyethylene glycol, 200 g of sorbitol, 0.5 g of eucalyptus oil, 0.5 g of sodium lauroyl sarcosinate, 0.5 g of trichlorogalactose, 0.5 g of stevioside, 0.0005 g of sunset yellow, 0.0005 g of gardenia yellow, 1 g of nipagin ester, and deionized water is added to make up to 1000 g.

[0176] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis comprises the following steps:

[0177] S1. The preparation method of the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil is as follows:

[0178] The Litsea cubeba volatile oil is included by β-cyclodextrin to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil for standby; specifically:

[0179] S11. Place the Litsea cubeba medicinal materials in a supercritical CO2 extraction kettle, cool CO2 to -4 °C, pump it into the system at a flow rate of 1.5 ml / min for extraction, the extraction temperature is 45 °C, the extraction pressure is 25 MPa, collect the extraction product, centrifuge, take the upper layer of oil liquid, and then dehydrate it with anhydrous sodium sulfate to obtain Litsea cubeba volatile oil.

[0180] S12. Dissolve the Litsea cubeba volatile oil in 95% ethanol in proportion to obtain a Litsea cubeba ethanol solution for standby.

[0181] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:0.4) into 20 times the amount of deionized water, heat it to 50 °C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 40 °C to obtain a β-cyclodextrin solution for standby.

[0182] S14. Add the Litsea cubeba ethanol solution into the β-cyclodextrin solution, mix evenly, freeze it in a -20 °C refrigerator for 10 h, take it out, and place it in a freeze dryer, and freeze-dry it at 40 °C for 20 h to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil.

[0183] The above-mentioned materials are made into toothpaste according to the following steps:

[0184] S2. Add Bletilla striata polysaccharide to 8 times the amount of deionized water, heat to 65 °C, and stir for 3.5 h to obtain an aqueous solution of Bletilla striata polysaccharide for later use.

[0185] S3. Dissolve trichlorogalactose, stevioside, eucalyptus oil, and nipagin ester in water, and mix with sorbitol and polyethylene glycol to obtain a mixed solution for later use.

[0186] S4. Mix the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, thickening silica, abrasive silica, and sodium lauroyl sarcosinate evenly to obtain a mixture for later use.

[0187] S5. Add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture, sunset yellow, and gardenia yellow to the paste-making tank in sequence, stir at a speed of 180 r / min for 80 min, evacuate the paste-making machine, and fill to obtain the toothpaste.

[0188] Example 11

[0189] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0190] 50 g of Bletilla striata polysaccharide, 100 g of β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, 15 g of thickening silica, 35 g of abrasive silica, 250 g of glycerol, 250 g of polyethylene glycol, 1 g of menthol, 15 g of sodium dodecyl sulfate, 1 g of xylitol, 1 g of stevioside, 0.02 g of lemon yellow, 1 g of sorbic acid, and make up to 1000 g with deionized water.

[0191] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0192] S1. The preparation method of the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil is as follows:

[0193] Use β-cyclodextrin to include Litsea cubeba volatile oil to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil for standby;

[0194] S11. Place the Litsea cubeba medicinal materials in a press, add a small amount of deionized water, squeeze out the volatile oil in the medicinal materials by mechanical extrusion, collect the squeezed oil-water mixture, centrifuge, take the upper layer of oil liquid, filter, and dehydrate with anhydrous sodium sulfate to obtain Litsea cubeba volatile oil.

[0195] S12. Dissolve the Litsea cubeba volatile oil in 95% ethanol according to a certain proportion to obtain a Litsea cubeba ethanol solution for later use.

[0196] S13. Take a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : mβ-环糊精 (ratio = 1:0.9) was added to 30 times the amount of deionized water and heated to 60 °C. After β-cyclodextrin was completely dissolved, the temperature was lowered to 50 °C to obtain a saturated aqueous solution of β-cyclodextrin for later use.

[0197] S14. The ethanol solution of Litsea cubeba was added to the saturated aqueous solution of β-cyclodextrin, mixed evenly, frozen in a refrigerator at -20 °C for 20 h, taken out, and placed in a freeze dryer for freeze-drying at 60 °C for 30 h to obtain the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil.

[0198] The above materials were made into toothpaste according to the following steps:

[0199] S2. Bletilla striata polysaccharide was added to 10 times the amount of deionized water and heated to 70 °C, stirred for 5 h to obtain an aqueous solution of Bletilla striata polysaccharide for later use.

[0200] S3. Xylitol, stevioside, menthol, and sorbic acid were dissolved in water and combined with polyethylene glycol and glycerol to obtain a mixed solution for later use.

[0201] S4. The β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, thickening silica, abrasive silica, and sodium lauryl sulfate were mixed evenly to obtain a mixture for later use.

[0202] S5. The aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture, and tartrazine were successively added to the paste-making tank, stirred at a speed of 160 r / min for 70 min, the paste-making machine was evacuated, and filled to obtain the toothpaste.

[0203] Example 12

[0204] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0205] 1 g of Bletilla striata polysaccharide, 5 g of the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil, 28 g of thickening silica, 42 g of abrasive silica, 300 g of sorbitol, 1 g of menthol, 12 g of sodium lauryl sulfate, 1.2 g of saccharin sodium, 0.002 g of tartrazine, 1 g of nipagin ester, and deionized water was added to make up to 1000 g.

[0206] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis includes the following steps:

[0207] S1. The preparation method of the β-cyclodextrin inclusion complex of Litsea cubeba volatile oil is as follows:

[0208] The β-cyclodextrin inclusion complex of Litsea cubeba volatile oil was obtained by encapsulating Litsea cubeba volatile oil with β-cyclodextrin and reserved; specifically:

[0209] S11. Place the cubeb fruits in a press, add a small amount of deionized water, and squeeze out the volatile oil from the herbs by mechanical pressing. Collect the squeezed oil-water mixture, centrifuge it, take the upper layer of oil, filter it, and then dehydrate it with anhydrous sodium sulfate to obtain cubeb volatile oil;

[0210] S12: Dissolve the cubeb volatile oil in 95% ethanol in proportion to obtain a cubeb ethanol solution for later use;

[0211] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄挥乙醇溶液 :m β-环糊精 = 1:0.1) to 10 times the amount of deionized water, heat it to 30°C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 20°C to obtain a β-cyclodextrin solution for later use.

[0212] S14. Add the cubeb ethanol solution to the β-cyclodextrin solution, mix them evenly in a high-pressure homogenizer, and then perform inclusion in a spray dryer (inlet temperature 80°C, outlet temperature 120°C) to obtain cubeb volatile oil β-cyclodextrin inclusion compound.

[0213] The above materials are made into toothpaste according to the following steps:

[0214] S2. Add bletilla striata polysaccharide to 7 times the amount of deionized water, heat it to 30°C, and stir for 1 h to obtain a bletilla striata polysaccharide aqueous solution for later use.

[0215] S3. Dissolve saccharin sodium, menthol, and nipagin ester in water and mix them with sorbitol to obtain a mixed solution for later use.

[0216] S4. Mix the cubeb volatile oil β-cyclodextrin inclusion compound, thickening silica, abrasive silica, and sodium lauryl sulfate evenly to obtain a mixture for later use.

[0217] S5. Add the bletilla striata polysaccharide aqueous solution, the mixed solution, the mixture, and tartrazine to the paste-making tank in sequence, stir at a speed of 20 r / min for 20 min, evacuate the paste-making machine, and fill it to obtain toothpaste.

[0218] Example 13

[0219] This example provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste includes the following components:

[0220] 2 g of bletilla striata polysaccharide, 6 g of cubeb volatile oil β-cyclodextrin inclusion compound, 25 g of thickening silica, 45 g of abrasive silica, 350 g of glycerol, 1.2 g of peppermint oil, 14 g of sodium lauroyl sarcosinate, 1.4 g of xylitol, 0.004 g of sunset yellow, 1 g of benzoic acid, and make up to 1000 g with deionized water.

[0221] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis, comprising the following steps:

[0222] S1. The preparation method of the piper cubeba volatile oil β-cyclodextrin clathrate is as follows:

[0223] The piper cubeba volatile oil is clathrated with β-cyclodextrin to obtain the piper cubeba volatile oil β-cyclodextrin clathrate for standby; specifically:

[0224] S11. Place the piper cubeba medicinal materials in a supercritical CO2 extraction kettle, cool CO2 to -4°C, pump it into the system at a flow rate of 1.5 ml / min for extraction, the extraction temperature is 45°C, the extraction pressure is 25 MPa, collect the extraction product, centrifuge, take the upper layer of oil liquid, and then dehydrate it with silica gel to obtain the piper cubeba volatile oil.

[0225] S12. Dissolve the piper cubeba volatile oil in 95% ethanol in proportion to obtain a piper cubeba ethanol solution for standby.

[0226] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 :m β-环糊精 = 1:0.2) to 6 times the amount of deionized water, heat it to 30°C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 20°C to obtain a β-cyclodextrin solution for standby.

[0227] S14. Add the piper cubeba ethanol solution to the β-cyclodextrin solution, mix it evenly in a high-pressure homogenizer, and perform clathration in a spray dryer (the inlet temperature is 50°C and the outlet temperature is 130°C) to obtain the piper cubeba volatile oil β-cyclodextrin clathrate.

[0228] The above materials are made into toothpaste according to the following steps:

[0229] S2. Add the bletilla striata polysaccharide to 8 times the amount of deionized water, heat it to 40°C, and stir for 2 h to obtain a bletilla striata polysaccharide aqueous solution for standby.

[0230] S3. Dissolve xylitol, peppermint oil, and benzoic acid in water and mix them with glycerol to obtain a mixed solution for standby;

[0231] S4. Mix the piper cubeba volatile oil β-cyclodextrin clathrate, thickening silica, friction silica, and sodium lauroyl sarcosinate evenly to obtain a mixture for standby;

[0232] S5. Add the bletilla striata polysaccharide aqueous solution, the mixed solution, the mixture, and sunset yellow to the paste-making tank in sequence, stir at a speed of 30 r / min for 30 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0233] Example 14

[0234] This embodiment provides a traditional Chinese medicine toothpaste for preventing and treating gingivitis. The traditional Chinese medicine toothpaste comprises the following components:

[0235] 4 g of bletilla striata polysaccharide, 8 g of β-cyclodextrin inclusion compound of cubeb fruit volatile oil, 44 g of thickening silica, 66 g of friction-type silica, 400 g of polyethylene glycol, 2 g of eucalyptus oil, 16 g of coconut oil amide propyl betaine, 1.6 g of trichlorogalactose, 0.006 g of gardenia yellow, 1 g of sorbic acid, and deionized water is added to make up to 1000 g.

[0236] A preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis comprises the following steps:

[0237] S1. The preparation method of the β-cyclodextrin inclusion compound of cubeb fruit volatile oil is as follows:

[0238] The cubeb fruit volatile oil is included with β-cyclodextrin to obtain the β-cyclodextrin inclusion compound of cubeb fruit volatile oil, and it is reserved for use; specifically:

[0239] S11. Place the cubeb fruit medicinal materials in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper layer of oil liquid, and then dehydrate it with anhydrous sodium sulfate to obtain cubeb fruit volatile oil.

[0240] S12. Dissolve the cubeb fruit volatile oil in 95% ethanol according to a ratio to obtain a cubeb fruit ethanol solution for use.

[0241] S13. Add a certain amount of β-cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 =1:0.4) to 4 times the amount of deionized water, heat to 30 °C, and after the β-cyclodextrin is completely dissolved, lower the temperature to 20 °C to obtain a β-cyclodextrin solution for use.

[0242] S14. Add the cubeb fruit ethanol solution to the β-cyclodextrin solution, mix well in a high-pressure homogenizer, and perform inclusion in a spray dryer (inlet temperature 100 °C, outlet temperature 100 °C) to obtain the β-cyclodextrin inclusion compound of cubeb fruit volatile oil.

[0243] The above materials are made into toothpaste according to the following steps:

[0244] S2. Add bletilla striata polysaccharide to 9 times the amount of deionized water, heat to 50 °C, and stir for 3 h to obtain a bletilla striata polysaccharide aqueous solution for use.

[0245] S3. Dissolve trichlorogalactose, eucalyptus oil, and sorbic acid in water, and mix with polyethylene glycol to obtain a mixed solution for use.

[0246] S4. Mix the betel pepper volatile oil β-cyclodextrin inclusion compound, thickening silica, friction silica, and cocamidopropyl betaine evenly to obtain a mixture for later use.

[0247] S5. Add the bletilla striata polysaccharide aqueous solution, mixed solution, mixture, and gardenia yellow into the paste-making tank in sequence, stir at a speed of 40 r / min for 40 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0248] Comparative Example 1

[0249] This comparative example provides a common toothpaste. The difference between this comparative example and Example 5 is that no bletilla striata polysaccharide and betel pepper volatile oil β-cyclodextrin inclusion compound are added. Specifically, the common toothpaste includes the following components:

[0250] 50 g of thickening silica, 100 g of friction silica, 480 g of sorbitol, 3 g of menthol, 20 g of sodium lauryl sulfate, 2 g of saccharin sodium, 0.01 g of tartrazine, 1 g of sorbic acid, and deionized water is added to make up to 1000 g.

[0251] The above materials are made into toothpaste according to the following steps:

[0252] S1. Dissolve saccharin sodium, menthol, and sorbic acid in water and mix with sorbitol for later use.

[0253] S2. Mix the thickening silica, friction silica, and sodium lauryl sulfate evenly for later use.

[0254] S3. Add the materials obtained in a and b and tartrazine into the paste-making tank in sequence, stir at a speed of 100 r / min for 50 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0255] Comparative Example 2

[0256] This comparative example provides a common traditional Chinese medicine toothpaste. The difference between this comparative example and Example 5 is that no betel pepper volatile oil β-cyclodextrin inclusion compound is added. Specifically, the common traditional Chinese medicine toothpaste includes the following components:

[0257] 8 g of bletilla striata polysaccharide, 50 g of thickening silica, 100 g of friction silica, 480 g of sorbitol, 3 g of menthol, 20 g of sodium lauryl sulfate, 2 g of saccharin sodium, 0.01 g of tartrazine, 0.1% of sorbic acid, and deionized water is added to make up to 1000 g.

[0258] A preparation method of a common traditional Chinese medicine toothpaste includes the following steps:

[0259] S1. Add bletilla striata polysaccharide into 10 times the amount of deionized water, heat to 50 °C, and stir for 5 h to obtain a bletilla striata polysaccharide aqueous solution for later use.

[0260] S2. Dissolve sodium saccharin, menthol, and sorbic acid in water, and mix with sorbitol to obtain a mixed solution for later use.

[0261] S3. Mix the β - cyclodextrin inclusion complex of cubeb volatile oil, thickening silica, friction silica, and sodium lauryl sulfate evenly to obtain a mixture for later use.

[0262] S5. Add the aqueous solution of bletilla striata polysaccharide, the mixed solution, the mixture, and tartrazine into the paste - making tank in sequence, stir at a speed of 100 r / min for 50 min, evacuate the paste - making machine, and then fill it to obtain the toothpaste.

[0263] Comparative Example 3

[0264] This comparative example provides a common traditional Chinese medicine toothpaste. The difference between this comparative example and Example 5 is that bletilla striata polysaccharide is not added. Specifically, the common traditional Chinese medicine toothpaste includes the following components:

[0265] β - cyclodextrin inclusion complex of cubeb volatile oil 12 g, thickening silica 50 g, friction silica 100 g, sorbitol 480 g, menthol 3 g, sodium lauryl sulfate 20 g, sodium saccharin 2 g, tartrazine 0.01 g, sorbic acid 0.1%, and deionized water is added to make up to 1000 g.

[0266] A preparation method of a common traditional Chinese medicine toothpaste includes the following steps:

[0267] S1. The preparation method of the β - cyclodextrin inclusion complex of cubeb volatile oil is as follows:

[0268] Use β - cyclodextrin to include cubeb volatile oil to obtain the β - cyclodextrin inclusion complex of cubeb volatile oil, and set it aside;

[0269] S11. Place cubeb medicinal materials in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper - layer oil liquid, and then dehydrate it with silica gel to obtain cubeb volatile oil.

[0270] S12. Dissolve the cubeb volatile oil in 95% ethanol to obtain a cubeb ethanol solution for later use.

[0271] S13. Add a certain amount of β - cyclodextrin (m 荜澄茄乙醇溶液 : m β-环糊精 = 1:0.5) to 25 times the amount of deionized water, heat to 50 °C, and after β - cyclodextrin is completely dissolved, lower the temperature to 40 °C to obtain a saturated aqueous solution of β - cyclodextrin for later use.

[0272] S14. Slowly drop the ethanol solution of Litsea cubeba oil into the saturated aqueous solution of β-cyclodextrin with stirring, perform inclusion for 3 h, place at 4 °C for 24 h, filter by suction while it is cold, and dry the precipitate at normal pressure at 40 °C for 3 hours to obtain the Litsea cubeba oil β-cyclodextrin inclusion compound.

[0273] The above materials are made into toothpaste according to the following steps:

[0274] S2. Dissolve sodium saccharin, menthol, and sorbic acid in water, and mix with sorbitol to obtain a mixed solution for later use.

[0275] S3. Mix the Litsea cubeba oil β-cyclodextrin inclusion compound, thickening silica, abrasive silica, and sodium lauryl sulfate evenly to obtain a mixture for later use.

[0276] S4. Add the mixed solution, the mixture, and tartrazine into the paste-making tank in sequence, stir at a speed of 100 r / min for 50 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0277] Comparative Example 4

[0278] This comparative example provides a traditional Chinese medicine toothpaste. The difference between this comparative example and Example 5 is that: the Litsea cubeba oil is not included. Specifically, the traditional Chinese medicine toothpaste includes the following components:

[0279] 8 g of Bletilla striata polysaccharide, 2 g of Litsea cubeba oil, 10 g of β-cyclodextrin, 50 g of thickening silica, 100 g of abrasive silica, 480 g of sorbitol, 3 g of menthol, 20 g of sodium lauryl sulfate, 2 g of sodium saccharin, 0.01 g of tartrazine, 0.1% of sorbic acid, and deionized water is added to make up to 1000 g.

[0280] A preparation method of a traditional Chinese medicine toothpaste includes the following steps:

[0281] S1. Preparation of Litsea cubeba oil

[0282] Place the Litsea cubeba medicinal materials in a flask, add an appropriate amount of deionized water, connect the volatile oil extraction device (light oil), heat to keep the solution in the flask slightly boiling, extract until the volatile oil in the collector no longer increases, release the liquid in the collector, centrifuge, take the upper layer of oil, and then dehydrate it with silica gel to obtain Litsea cubeba oil.

[0283] S2. Add Bletilla striata polysaccharide to 10 times the amount of deionized water, heat to 50 °C, and stir for 5 h to obtain an aqueous solution of Bletilla striata polysaccharide for later use.

[0284] S3. Dissolve sodium saccharin, menthol, and sorbic acid in water, and mix with sorbitol to obtain a mixed solution for later use.

[0285] S4. Mix the volatile oil of Litsea cubeba, β-cyclodextrin, thickening silica, friction silica, and sodium dodecyl sulfate evenly to obtain a mixture for later use.

[0286] S5. Add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture, and tartrazine into the paste-making tank in sequence, stir at a speed of 100 r / min for 50 min, evacuate the paste-making machine, and fill it to obtain the toothpaste.

[0287] Application Example 1

[0288] Efficacy Evaluation

[0289] 1. Experimental materials: Toothpastes prepared in Comparative Example 1, Comparative Example 2, Comparative Example 3, Comparative Example 4, and Example 5.

[0290] 2. Test subjects: 150 subjects were selected. The inclusion criteria for the subjects were: good overall health, no important systemic diseases, more than 20 detectable teeth, aged 18 - 70 years old; if female, not in pregnancy and lactation; the subjects should have an appropriate degree of dental plaque or gingivitis; not participating in other similar experimental studies simultaneously; signing the informed consent form and being able to complete the clinical trial as required. Patients with a history of allergy to the components of the test toothpaste, currently taking drugs that affect the test results, using antibiotics one month before participating in the study, having open dental caries or mucosal lesions in the oral cavity, and suffering from severe periodontitis were excluded from this study.

[0291] 3. Test method: The subjects were randomly divided into 6 groups, with 30 subjects in each group. There were no significant differences in gender, age, and general information among the subjects in each group. Before the start of the experiment, the patients needed to receive oral hygiene education, remove dental plaque, polish tooth enamel, and remove obvious large tartar, learn the Bass brushing method, and uniformly use the toothpaste of Comparative Example 1 for 2 weeks to adjust the baseline level to be consistent. Experimental group 1 used the toothpaste of Comparative Example 2, experimental group 2 used the toothpaste of Comparative Example 3, experimental group 3 used the toothpaste of Comparative Example 4, experimental group 4 used the toothpaste of Example 5, and the control group used the toothpaste of Comparative Example 1. Each group used the corresponding toothpaste once in the morning and evening every day, taking an amount the size of a soybean each time, and using the Bass brushing method for 3 minutes continuously for 12 weeks. After continuous use for 12 weeks, the subjects in each group could not replace other oral cleaning products during the test period, and follow-up was conducted at baseline, 4 weeks, 8 weeks, and 12 weeks.

[0292] 4. Analysis of test results

[0293] (1) Plaque Index (PLI): Scoring is based on the thickness of plaque on the tooth surface rather than the coverage area. If there is no plaque in the gingival margin area, it is 0 points. If there is a thin layer of plaque on the tooth surface in the gingival margin area but it is not visible upon visual inspection, and plaque can be seen when the tip of a probe is used to scrape the tooth surface, it is 1 point. If moderate amounts of plaque are visible at the gingival margin or adjacent surfaces, it is 2 points. If there is a large amount of soft dirt in the gingival sulcus or gingival margin area and adjacent surfaces, it is 3 points.

[0294] (2) Gingival Index Score (BI): 0 indicates healthy gums with no inflammation or bleeding. 1 represents inflammatory changes in the color of the gums with no bleeding upon probing. 2 indicates punctate bleeding after probing. 3 represents bleeding spreading along the gingival margin upon probing. 4 represents bleeding filling and overflowing from the gingival sulcus. 5 represents spontaneous bleeding.

[0295] 5. The experimental results are shown in the following table:

[0296] Table 1 Comparison of plaque index before and after use in each group of subjects

[0297]

[0298] Table 2 Comparison of gingival index before and after use in each group of subjects

[0299]

[0300]

[0301] For the efficacy evaluation experiment of the toothpaste of the present invention, as can be seen from Table 1, in experimental group 4, after using the toothpaste of Example 5 for 8 weeks, the PLI had a significant decrease compared with the baseline level (P < 0.05). After using it for 12 weeks, the PLI further decreased (P < 0.001), and there was also a statistical difference between 4 weeks and 12 weeks (P < 0.001). And since the 8th week in experimental group 4, its plaque index was significantly lower than that of other experimental groups, indicating that the combined application of polysaccharide from Bletilla striata and β - cyclodextrin inclusion complex of volatile oil from Litsea cubeba is superior to the single use in inhibiting plaque formation, and the volatile oil from Litsea cubeba can better exert its efficacy after being included by β - cyclodextrin. The control group used the toothpaste of Comparative Example 1, and although the PLI showed a downward trend before and after use, there was no obvious statistical difference.

[0302] For the efficacy evaluation experiment of the toothpaste of the present invention, as can be seen from Table 2, when the toothpaste of Example 5 was used by Experimental Group 4 for 12 weeks, the BI showed a significant decrease compared with the baseline level (P < 0.001), and there were statistical differences in BI between 12 weeks and 4 weeks, 8 weeks (P < 0.001). At 12 weeks, the BI of Experimental Group 4 was significantly lower than that of Experimental Group 1 and Experimental Group 2, indicating that the combined application of polysaccharide from Bletilla striata and β-cyclodextrin inclusion complex of volatile oil from Litsea cubeba was significantly superior to the single use in eliminating gingival inflammation and improving gingival bleeding, and the volatile oil from Litsea cubeba could better exert its efficacy after being included by β-cyclodextrin. However, there was no obvious downward trend in the control group before and after using the toothpaste of Comparative Example 1, and there were no significant differences in statistical analysis.

[0303] Application Example 2

[0304] After storing the toothpastes prepared in Comparative Examples 1 to 4 and Example 5 at 25°C ± 2°C and 60% ± 10% humidity for 90 days, take them out and retest the plaque index (PLI) and gingival index score (BI) according to the method of Application Example 1. The test results are shown in Table 3 and Table 4.

[0305] The change ratio of plaque index before and after storage = (plaque index after storage - plaque index before storage) / plaque index before storage × 100%.

[0306] The change ratio of gingival index before and after storage = (gingival index after storage - gingival index before storage) / gingival index before storage × 100%.

[0307] Table 3 Comparison of plaque index before and after use of each group of subjects after storage

[0308]

[0309] Table 4 Comparison of gingival index before and after use of each group of subjects after storage

[0310]

[0311] For the stability evaluation experiment of the toothpaste of the present invention, as can be seen from Table 3 and Table 4, the change ratios of plaque index and gingival index of Experimental Group 3 after 12 weeks were much larger than those of other experimental groups and the control group, and there were statistical differences (P < 0.001), indicating that the volatile oil from Litsea cubeba without inclusion directly added to the toothpaste would lose its efficacy during long-term storage, affecting the storage period of the toothpaste. In addition, during the experiment, it was found that when the volatile oil from Litsea cubeba without inclusion was directly added to the toothpaste, in the long-term stability experiment, the phenomenon of oil-water separation of the paste body would occur, affecting the normal use of the toothpaste.

[0312] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit them. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions of the present invention or make equivalent replacements, and these modifications or equivalent replacements cannot make the modified technical solutions deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A traditional Chinese medicine toothpaste for preventing and treating gingivitis, characterized in that: The traditional Chinese medicine toothpaste comprises the following components by mass fraction: Bletilla striata polysaccharide 0.05 - 5%, β - cyclodextrin inclusion compound of Litsea cubeba volatile oil 0.1 - 10%, silicon dioxide 5 - 30%, humectant 30 - 70%, fragrance 0.05 - 0.5%, foaming agent 0.05 - 5%, sweetener 0.1 - 1%, colorant 0.0001 - 0.5%, preservative 0.1%, and the balance being deionized water.

2. The traditional Chinese medicine toothpaste for preventing and treating gingivitis according to claim 1, wherein: The traditional Chinese medicine toothpaste comprises the following components by mass fraction: Bletilla striata polysaccharide 0.3 - 1.3%, β - cyclodextrin inclusion compound of Litsea cubeba volatile oil 0.7 - 1.7%, silicon dioxide 10 - 20%, humectant 45 - 55%, fragrance 0.2 - 0.3%, foaming agent 1.5 - 2.5%, sweetener 0.1 - 0.3%, colorant 0.0005 - 0.0015%, preservative 0.1%, and the balance being deionized water.

3. The Chinese medicinal toothpaste for preventing and treating gingivitis according to claim 1, wherein: The silicon dioxide includes at least one of thickening silicon dioxide and friction silicon dioxide.

4. The Chinese medicinal toothpaste for preventing and treating gingivitis according to claim 1, wherein: The purity of Bletilla striata polysaccharide is 10% - 90%; the humectant is selected from at least one of sorbitol, polyethylene glycol, glycerol and propylene glycol; the fragrance is selected from at least one of menthol, peppermint oil and eucalyptus oil; the foaming agent is selected from at least one of sodium dodecyl sulfate, sodium lauroyl sarcosinate and cocamidopropyl betaine; the sweetener is selected from at least one of sodium saccharin, trichlorogalactose, stevioside and xylitol; the colorant is selected from at least one of sunset yellow, lemon yellow, gardenia yellow and safflower yellow; the preservative is selected from at least one of parabens, benzoic acid and sorbic acid.

5. The preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis according to any one of claims 1 to 4, characterized in that: It includes the following steps: S1: Inclusion - complex the Litsea cubeba volatile oil with β - cyclodextrin to obtain the β - cyclodextrin inclusion compound of Litsea cubeba volatile oil, and set aside; S2: Add deionized water to Bletilla striata polysaccharide, heat and stir to obtain an aqueous solution of Bletilla striata polysaccharide; S3: Dissolve the sweetener, fragrance and preservative in water, and mix with the humectant to obtain a mixed solution, and set aside; S4: Mix the β - cyclodextrin inclusion compound of Litsea cubeba volatile oil, silicon dioxide and foaming agent evenly to obtain a mixture, and set aside; S5: Add the aqueous solution of Bletilla striata polysaccharide, the mixed solution, the mixture and the colorant to the paste - making tank in sequence, stir evenly, evacuate the paste - making machine, and fill to obtain the traditional Chinese medicine toothpaste.

6. The preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis according to claim 5, characterized in that: In step S1, the specific preparation process of the β - cyclodextrin inclusion compound of Litsea cubeba volatile oil is as follows: S11: Extract the Litsea cubeba volatile oil from the Litsea cubeba raw material, and set aside; S12: Dissolve the Litsea cubeba volatile oil in 95% ethanol to obtain a Litsea cubeba ethanol solution, and set aside; S13: Add deionized water to β - cyclodextrin, mix evenly to obtain a β - cyclodextrin solution, and set aside; S14: Add the Litsea cubeba ethanol solution to the β - cyclodextrin solution, carry out inclusion - complexation, then stand, filter and dry to obtain the β - cyclodextrin inclusion compound of Litsea cubeba volatile oil.

7. The preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis according to claim 6, characterized in that: In step S11, the method for extracting Litsea cubeba volatile oil is one of steam distillation method, supercritical fluid extraction method or pressing method. After extraction, it is dehydrated with anhydrous sodium sulfate or silica gel to obtain Litsea cubeba volatile oil.

8. The preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis according to claim 7, characterized in that: In step S12, the mass ratio of Litsea cubeba volatile oil to 95% ethanol is 1:0.1 - 2; In step S13, add 10 to 40 times deionized water to β-cyclodextrin, heat to 30 to 70 °C, and after β-cyclodextrin is completely dissolved, cool to 20 to 60 °C to obtain a β-cyclodextrin solution.

9. The preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis according to claim 7, characterized in that: In step S14, the inclusion time is 1 to 5 h; the static temperature is 4 to 8 °C, and the static time is 10 to 30 h; the drying temperature is 20 to 60 °C, and the drying time is 1 to 10 h.

10. The preparation method of a traditional Chinese medicine toothpaste for preventing and treating gingivitis according to claim 5, characterized in that: In step S2, add 7 to 13 times deionized water to Bletilla striata polysaccharide, heat to 30 to 70 °C, and stir for 1 to 10 h to obtain an aqueous solution of Bletilla striata polysaccharide; In step S5, the stirring speed is 20 to 180 r / min, and the stirring time is 20 to 80 min.

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