Chinese herbal medicine toothpaste formula and preparation method thereof

Abstract

The invention relates to the technical field of toothpaste preparation, and particularly discloses a Chinese herbal medicine toothpaste formula and a preparation method thereof, the Chinese herbal medicine toothpaste formula comprises the following raw materials by weight: 17-18 parts of a functional component, 2.4-2.8 parts of a slow release synergist, 20-22 parts of a friction agent, 28-32 parts of a humectant, 2.6-3.4 parts of a surfactant, 0.16-0.18 part of a preservative, 1.8-2 parts of a thickener, 1.4-1.6 parts of essence, 5.8-6.2 parts of a flavoring agent and 16-18 parts of deionized water; taxillus sutchuenensis, herba cepbalanoplosis segeti, plantain herb, herba pyrolae and fructus forsythiae are used as core materials of functional components, gelatin and modified sodium alginate are used as wall materials, the functional components are prepared, and a slow-release synergist containing anthocyanin, bromelain and rhamnolipid is added, so that the effects of removing stains and whitening skin are achieved; moreover, release of quercetin, quercitrin and other components in the traditional Chinese medicine extract is promoted, and the anti-inflammatory, bleeding-stopping, halitosis-removing, stain-removing and whitening effects of the toothpaste are improved.

Description

TECHNICAL FIELD

[0001] The application relates to the toothpaste preparation technical field, in particular to a Chinese herbal medicine toothpaste formula and a preparation method thereof. BACKGROUND

[0002] As a special group, the oral health of the elderly faces unprecedented challenges. Long-term wear and tear and acid erosion of the teeth of the elderly, as well as inevitable oral diseases such as gum atrophy, tooth root exposure and periodontal disease with age, are the essential causes of the elderly being susceptible to pain when encountering external stimuli. At the same time, many elderly people have decreased recovery ability and poor drug absorption, which often leads to long-term treatment and repeated treatment of elderly patients in clinical practice, thereby increasing the pain of the elderly. Therefore, it is particularly important to use a specific nursing toothpaste to nurse the oral cavity of the elderly in the form of tooth brushing.

[0003] Compared with the oral cavity of young people, the oral cavity of the elderly is more prone to problems such as soreness, odor, bleeding and long bubble due to heat. Therefore, completely using the existing toothpaste formula or the toothpaste formula for young people will greatly reduce the effect of the elderly nursing toothpaste.

[0004] Based on the above defects, the application provides a Chinese herbal medicine toothpaste formula and a preparation method thereof. SUMMARY

[0005] In order to solve the problems mentioned in the background, the application provides a Chinese herbal medicine toothpaste formula and a preparation method thereof.

[0006] A Chinese herbal medicine toothpaste formula comprises the following raw materials in parts by weight: 17-18 parts of efficacy components, 2.4-2.8 parts of slow-release synergists, 20-22 parts of abrasives, 28-32 parts of humectants, 2.6-3.4 parts of surfactants, 0.16-0.18 parts of preservatives, 1.8-2 parts of thickening agents, 1.4-1.6 parts of fragrances, 5.8-6.2 parts of flavoring agents and 16-18 parts of deionized water. The preparation method of the Chinese herbal medicine toothpaste comprises the following steps: The thickening agent, the humectant, the flavoring agent and the deionized water are mixed and stirred uniformly, the abrasive and the surfactant are added and stirred uniformly in a vacuum, the efficacy component, the slow-release synergist, the fragrance and the preservative are further added and stirred uniformly, the vacuum is maintained, the bubble is extracted for 6-10 minutes, the material is discharged, the toothpaste is filled and packaged, and the Chinese herbal medicine toothpaste is obtained.

[0007] Preferably, the abrasive is nano-hydroxyapatite or calcium hydrogen phosphate.

[0008] Preferably, the humectant is glycerol or propylene glycol.

[0009] Preferably, the surfactant is sodium lauryl ether sulphate or cocamidopropyl betaine.

[0010] Preferably, the preservative is nipagin or sodium benzoate.

[0011] Preferably, the thickening agent is xanthan gum or carrageenan.

[0012] Preferably, the flavoring agent is peppermint or spearmint.

[0013] Preferably, the flavoring agent is D-sorbitol or xylitol.

[0014] Preferably, the functional ingredient is prepared by the following steps: Step A1, mix sodium alginate and deionized water, stir evenly at room temperature, adjust the pH value to 8-9, then add dropwise the mixed solution a of octenyl succinic anhydride and isopropyl alcohol, control the droping within 10 min, after dropping, increase the temperature to 68-72℃, stir for 4-6h, then adjust the pH value to 6.4-6.8, wash, dry, obtain modified sodium alginate, wherein the mass ratio of sodium alginate, deionized water and mixed solution a is 4.6-5.4:96-108:20, the mass ratio of octenyl succinic anhydride and isopropyl alcohol in the mixed solution a is 1.2-2.2:60, in the above reaction process, ring-opening esterification reaction occurs between sodium alginate and octenyl succinic anhydride, and the modified sodium alginate is obtained; Step A2, at room temperature, add gelatin aqueous solution and modified sodium alginate aqueous solution into anhydrous ethanol, stir evenly, add Chinese medicine extract and zinc lactate while stirring, increase the temperature to 62-66℃, emulsify for 12-16 min, adjust the pH to 4.2-4.4, decrease the temperature to 6-10℃, then adjust the pH to 8.8-9.2, stand, separate the layers, centrifuge, dry, obtain the functional ingredient, wherein the mass ratio of gelatin aqueous solution, modified sodium alginate aqueous solution, anhydrous ethanol, Chinese medicine extract and zinc lactate is 3-5:1.2-1.6:50-60:3.6-5.4:0.6-0.8, in the above process, the functional ingredient is prepared by complex coacervation method with gelatin and modified sodium alginate as wall material and Chinese medicine extract and zinc lactate as core material.

[0015] Preferably, the mass fraction of the gelatin aqueous solution is 0.8-1.2%.

[0016] Preferably, the mass fraction of the modified sodium alginate aqueous solution is 4.6-5.4%.

[0017] Preferably, the Chinese medicine extract is prepared by the following steps: Step B1, the morus alba, herba, plantago, peduncle and forsythia are ground together, passed through a 60-100 mesh sieve, soaked in deionized water for 3-5 hours, anhydrous ethanol is added, refluxed and extracted 1-3 times, filtered while hot, and the filtrate is collected, wherein the mass ratio of morus alba, herba, plantago, peduncle, forsythia, deionized water and anhydrous ethanol is 4.2-5.6:2.8-3.4:3.6-4.4:3.2-3.6:2.2-2.4:160-220:120-150; Step B2, the filtrate in step B1 is concentrated under reduced pressure until the anhydrous ethanol is completely volatilized, and the concentrated solution is collected; Step B3, the concentrated solution in step B2 is diluted with deionized water, placed for 4-6 hours, centrifuged to obtain the supernatant, concentrated to a thick paste with a relative density of 1.2-1.3 at 80℃, dried at 60-70℃, ground to 120-160 mesh, and the traditional Chinese medicine extract is obtained, wherein the mass ratio of the concentrated solution and deionized water is 1:4-5.

[0018] Preferably, the slow-release synergist is prepared by the following steps: Anthocyanins, bromelain and rhamnolipid are added to phosphate buffer, heated to 46-52℃, stirred for 14-18min, and the slow-release synergist is obtained, wherein the mass ratio of anthocyanins, bromelain, rhamnolipid and phosphate buffer is 0.8-1.2:0.2-0.4:0.04-0.06:40-50.

[0019] Compared with the prior art, the present application has the following beneficial effects: The functional component core material of the present application is prepared from morus alba, herba, plantago, peduncle and forsythia and zinc lactate, wherein morus alba and forsythia have anti-inflammatory and antibacterial effects, which are suitable for toothpaste, herba, plantago and peduncle have anti-inflammatory effects, and peduncle also has anti-allergic and deodorizing effects, and zinc lactate releases zinc ions with antibacterial effect during preparation, and through the synergistic effect of them, the prepared toothpaste has anti-inflammatory, hemostatic and deodorizing effects, the wall material is prepared by blending modified sodium alginate and gelatin, which not only has good water solubility and dissolves rapidly during brushing to release the wrapped traditional Chinese medicine extract in time to play the effects of anti-inflammatory, hemostatic and deodorizing, but also the modified sodium alginate has emulsifying effect, which improves the compatibility between the functional components, the slow-release synergist and other components, and further improves the effects of anti-inflammatory, hemostatic and deodorizing.

[0020] The Chinese herbal toothpaste disclosed in the application adds a slow-release synergist in the preparation process, the slow-release synergist contains anthocyanins, bromelain and rhamnolipid, the presence of anthocyanins and bromelain not only can play the role of stain removal and whitening, but also can promote the release of active ingredients such as quercetin and quercitrin in the traditional Chinese medicine extract, further improving the effects of anti-inflammatory, hemostasis, deodorization, stain removal and whitening. DETAILED DESCRIPTION

[0021] In order to make the embodiments of the application easier to understand, the application will be described in detail below in combination with specific examples, which only serve to illustrate the application and are not limited to the application.

[0022] The main raw materials used in the examples and comparative examples and the content of the components are shown as follows: The phosphate buffer is Sorensen phosphate buffer commercially available from Shanghai Yuan Ye Biological Technology Co., Ltd., model R27148, product specification 0.01 mol / L, pH 7.4, the sodium alginate is commercially available from Leshengyuan Biological Technology (Nanjing) Co., Ltd., CAS No. 9005-38-3, and the gelatin is commercially available from Shandong Xinxiong Biological Technology Co., Ltd., CAS No. 9000-70-8.

[0023] The application will be further described in detail below in combination with examples and comparative examples.

[0024] Preparation Examples 1-3 and Comparative Preparation Examples 1-3 provide a preparation method of the traditional Chinese medicine extract.

[0025] Preparation Example 1 The preparation example provides a traditional Chinese medicine extract prepared by the following steps: Step B1, morinda officinalis, radix erigerontis, plantain, pedunculate eriodictyon and forsythia are ground together, passed through a 60-mesh sieve, soaked in deionized water for 3 h, anhydrous ethanol is added, reflux extraction is performed, and the filtrate is collected while hot, wherein the mass ratio of morinda officinalis, radix erigerontis, plantain, pedunculate eriodictyon, forsythia, deionized water and anhydrous ethanol is 4.2:2.8:3.6:3.2:2.2:160:120; Step B2, the filtrate in step B1 is concentrated under reduced pressure until the anhydrous ethanol is completely volatilized, and the concentrated solution is collected; Step B3, the concentrated solution in step B2 is diluted with deionized water, and the mixture is allowed to stand for 4 h, the supernatant is taken by centrifugation, and the supernatant is concentrated to a thick paste with a relative density of 1.2 at 80°C, dried at 60°C, and ground into 120 mesh to obtain a traditional Chinese medicine extract, wherein the mass ratio of the concentrated solution and deionized water is 1:4.

[0026] Preparation Example 2 The preparation example provides a traditional Chinese medicine extract prepared by the following steps: Step B1, morus, small chrysanthemum, plantain, deerweed and forsythia are co-ground, passed through a 80 mesh sieve, soaked in deionized water for 4h, anhydrous ethanol is added, reflux extraction, filter while hot, collect the filtrate, wherein the mass ratio of morus, small chrysanthemum, plantain, deerweed, forsythia, deionized water and anhydrous ethanol is 4.9:3.1:4.0:3.4:2.3:190:135; Step B2, the filtrate in step B1 is concentrated under reduced pressure until the anhydrous ethanol is completely volatilized, and the concentrated solution is collected; Step B3, the concentrated solution in step B2 is diluted with deionized water, placed for 5h, centrifuged to take the supernatant, concentrated to a thick paste with a relative density of 1.25 at 80℃, dried at 65℃, and ground into 140 mesh to obtain a traditional Chinese medicine extract, wherein the mass ratio of the concentrated solution and deionized water is 1:4.5.

[0027] Preparation Example 3 The present preparation example provides a traditional Chinese medicine extract prepared by the following steps: Step B1, morus, small chrysanthemum, plantain, deerweed and forsythia are co-ground, passed through a 80 mesh sieve, soaked in deionized water for 4h, anhydrous ethanol is added, reflux extraction, filter while hot, collect the filtrate, wherein the mass ratio of morus, small chrysanthemum, plantain, deerweed, forsythia, deionized water and anhydrous ethanol is 4.9:3.1:4.0:3.4:2.3:190:135; Step B2, the filtrate in step B1 is concentrated under reduced pressure until the anhydrous ethanol is completely volatilized, and the concentrated solution is collected; Step B3, the concentrated solution in step B2 is diluted with deionized water, placed for 5h, centrifuged to take the supernatant, concentrated to a thick paste with a relative density of 1.25 at 80℃, dried at 65℃, and ground into 140 mesh to obtain a traditional Chinese medicine extract, wherein the mass ratio of the concentrated solution and deionized water is 1:4.5.

[0028] Comparative Preparation Example 1 The present preparation example provides a traditional Chinese medicine extract prepared by the following steps: Step B1, morus, small chrysanthemum, plantain, deerweed and forsythia are co-ground, passed through a 80 mesh sieve, soaked in deionized water for 4h, anhydrous ethanol is added, reflux extraction, filter while hot, collect the filtrate, wherein the mass ratio of morus, small chrysanthemum, plantain, deerweed, forsythia, deionized water and anhydrous ethanol is 4.9:3.1:4.0:3.4:2.3:190:135; Step B2, the filtrate in step B1 is concentrated under reduced pressure until the anhydrous ethanol is completely volatilized, and the concentrated solution is collected; Step B3, the concentrated solution in step B2 is diluted by adding deionized water, and is left to stand for 4h, and the supernatant is taken by centrifugation, and is concentrated to a thick paste with a relative density of 1.2 at 80℃, and is dried at 60℃, and is crushed to 120 mesh to obtain the traditional Chinese medicine extract, wherein the mass ratio of the concentrated solution to the deionized water is 1:4.

[0029] Comparative Preparation Example 2 The present comparative preparation example provides a traditional Chinese medicine extract prepared by the following steps: Step B1, the Morinda officinalis, the Herba Spigelia, the Plantago asiatica and the Forsythia suspensa are ground together, and are passed through a 60 mesh sieve, and are soaked in deionized water for 3h, and anhydrous ethanol is added, and is refluxed to extract, and is filtered while hot, and the filtrate is collected, wherein the mass ratio of the Morinda officinalis, the Herba Spigelia, the Plantago asiatica, the Forsythia suspensa, the deionized water and the anhydrous ethanol is 4.2:2.8:3.2:2.2:160:120; Step B2, the filtrate in step B1 is concentrated under reduced pressure until the anhydrous ethanol is completely volatilized, and the concentrated solution is collected; Step B3, the concentrated solution in step B2 is diluted by adding deionized water, and is left to stand for 4h, and the supernatant is taken by centrifugation, and is concentrated to a thick paste with a relative density of 1.2 at 80℃, and is dried at 60℃, and is crushed to 120 mesh to obtain the traditional Chinese medicine extract, wherein the mass ratio of the concentrated solution to the deionized water is 1:4.

[0030] Preparation Examples 4-6 and Comparative Preparation Examples 3-6 provide an efficacy component.

[0031] Preparation Example 4 The present preparation example provides an efficacy component prepared by the following steps: Step A1, sodium alginate and deionized water are mixed, and are stirred at room temperature at a rotation speed of 460rpm for 12min until uniform, and the pH value is adjusted to 8 with a 5% sodium carbonate aqueous solution, and a mixed solution a of octenyl succinic anhydride and isopropyl alcohol is added dropwise, and the dropping is completed within 10min, and after the dropping is completed, the temperature is raised to 68℃, and stirring is carried out for 4h, and the pH value is adjusted to 6.4 with a 1% citric acid aqueous solution, and is washed with anhydrous ethanol and deionized water for 3 times respectively, and is dried at 56℃ until the weight is constant to obtain modified sodium alginate, wherein the mass ratio of the sodium alginate, the deionized water and the mixed solution a is 4.6:96:20, and in the mixed solution a, the mass ratio of the octenyl succinic anhydride to the isopropyl alcohol is 1.2:60; Step A2, at room temperature, 0.8% gelatin aqueous solution and 4.6% modified sodium alginate aqueous solution were added into anhydrous ethanol, stirred at 520 rpm for 14 min until uniform, while stirring, the extract of traditional Chinese medicine prepared in Preparation Example 1 and zinc lactate were added, the temperature was raised to 62℃, the stirring speed was adjusted to 1100 rpm, and the emulsification reaction was continued for 12 min, 0.6% acetic acid aqueous solution was used to adjust the pH to 4.2, the temperature was lowered to 6℃, 2.0% sodium carbonate aqueous solution was used to adjust the pH to 8.8, and then it was left to stand, separated, centrifuged, and dried at 54℃ until constant weight to obtain the functional ingredient, wherein the mass ratio of gelatin aqueous solution, modified sodium alginate aqueous solution, anhydrous ethanol, traditional Chinese medicine extract and zinc lactate was 3:1.2:50:3.6:0.6.

[0032] Preparation Example 5 The present preparation example provides a functional ingredient, which is prepared by the following steps: Step A1, sodium alginate and deionized water were mixed, stirred at room temperature and a stirring speed of 500 rpm for 15 min until uniform, 7.5% sodium carbonate aqueous solution was used to adjust the pH to 8.5, and then the mixed solution a of octenyl succinic anhydride and isopropyl alcohol was added dropwise, which was controlled to be completed within 10 min, after dropping, the temperature was raised to 70℃, and the stirring reaction was continued for 5 h, 2% citric acid aqueous solution was used to adjust the pH to 6.6, and then anhydrous ethanol and deionized water were used for washing respectively for 4 times, and dried at 60℃ until constant weight to obtain the modified sodium alginate, wherein the mass ratio of sodium alginate, deionized water and mixed solution a was 5.0:102:20, and the mass ratio of octenyl succinic anhydride and isopropyl alcohol in the mixed solution a was 1.7:60; Step A2, at room temperature, 1.0% gelatin aqueous solution and 5.0% modified sodium alginate aqueous solution were added into anhydrous ethanol, stirred at 540 rpm for 12 min until uniform, while stirring, the extract of traditional Chinese medicine prepared in Preparation Example 2 and zinc lactate were added, the temperature was raised to 64℃, the stirring speed was adjusted to 1200 rpm, and the emulsification reaction was continued for 14 min, 0.5% acetic acid aqueous solution was used to adjust the pH to 4.3, the temperature was lowered to 8℃, 2.2% sodium carbonate aqueous solution was used to adjust the pH to 9, and then it was left to stand, separated, centrifuged, and dried at 56℃ until constant weight to obtain the functional ingredient, wherein the mass ratio of gelatin aqueous solution, modified sodium alginate aqueous solution, anhydrous ethanol, traditional Chinese medicine extract and zinc lactate was 4:1.4:55:4.5:0.7.

[0033] Preparation Example 6 The present preparation example provides a functional ingredient, which is prepared by the following steps: Step A1, mix sodium alginate and deionized water, stir at room temperature and a speed of 540 rpm for 18 min until uniform, adjust the pH to 9 with a 10% sodium carbonate solution, then add dropwise a mixture a of octenyl succinic anhydride and isopropyl alcohol, control the dropwise addition to be completed within 10 min, after the dropwise addition, increase the temperature to 72℃, stir for 6 h, adjust the pH to 6.8 with a 1% citric acid solution, wash with anhydrous ethanol and deionized water for 5 times each, dry at 64℃ until constant weight, to obtain modified sodium alginate, wherein the mass ratio of sodium alginate, deionized water and mixture a is 5.4:108:20, and the mass ratio of octenyl succinic anhydride and isopropyl alcohol in mixture a is 2.2:60; Step A2, at room temperature, add a 1.2% gelatin aqueous solution and a 5.4% modified sodium alginate aqueous solution into anhydrous ethanol, stir until uniform, add the traditional Chinese medicine extract prepared in Preparation Example 3 and zinc lactate while stirring, increase the temperature to 66℃, emulsify for 16 min, adjust the pH to 4.4 with a 0.4% acetic acid solution, decrease the temperature to 10℃, then adjust the pH to 9.2 with a 2.4% sodium carbonate solution, stand, separate the layers, centrifuge, dry at 58℃ until constant weight, to obtain the functional ingredient, wherein the mass ratio of the gelatin aqueous solution, the modified sodium alginate aqueous solution, the anhydrous ethanol, the traditional Chinese medicine extract and the zinc lactate is 5:1.6:60:5.4:0.8.

[0034] Comparative Preparation Example 3 This comparative preparation example provides a functional ingredient, which is prepared by the following steps: Step A1, mix sodium alginate and deionized water, stir at room temperature and a speed of 460 rpm for 12 min until uniform, adjust the pH to 8 with a 5% sodium carbonate solution, then add dropwise a mixture a of octenyl succinic anhydride and isopropyl alcohol, control the dropwise addition to be completed within 10 min, after the dropwise addition, increase the temperature to 68℃, stir for 4 h, then adjust the pH to 6.4 with a 1% citric acid solution, wash with anhydrous ethanol and deionized water for 3 times each, dry at 56℃ until constant weight, to obtain modified sodium alginate, wherein the mass ratio of sodium alginate, deionized water and mixture a is 4.6:96:20, and the mass ratio of octenyl succinic anhydride and isopropyl alcohol in mixture a is 1.2:60; Step A2, at room temperature, the 0.8% gelatin aqueous solution and the modified sodium alginate aqueous solution were added into anhydrous ethanol, stirred at 520 rpm for 14 min until uniform, the Chinese medicine extract and zinc lactate prepared in Comparative Preparation Example 1 were added while stirring, the temperature was raised to 62℃, the stirring speed was adjusted to 1100 rpm, and the emulsification reaction was continued for 12 min, the pH was adjusted to 4.2 with 0.6% acetic acid aqueous solution, the temperature was lowered to 6℃, the pH was adjusted to 8.8 with 2.0% sodium carbonate aqueous solution, and then it was left to stand, separated, centrifuged, and dried at 54℃ until constant weight to obtain the functional ingredient, wherein the mass ratio of the gelatin aqueous solution, the modified sodium alginate aqueous solution, the anhydrous ethanol, the Chinese medicine extract and the zinc lactate was 3:1.2:50:3.6:0.6.

[0035] Comparative Preparation Example 4 The present comparative preparation example provides a functional ingredient, which is prepared by the following steps: Step A1, sodium alginate and deionized water were mixed, stirred at room temperature and a stirring speed of 460 rpm for 12 min until uniform, the pH value was adjusted to 8 with 5% sodium carbonate aqueous solution, and then the mixed solution a of octenyl succinic anhydride and isopropyl alcohol was added dropwise, which was controlled to be completed within 10 min, after dropping, the temperature was raised to 68℃, and the stirring reaction was continued for 4 h, then the pH value was adjusted to 6.4 with 1% citric acid aqueous solution, and then the modified sodium alginate was obtained by washing with anhydrous ethanol and deionized water for 3 times respectively and drying at 56℃ until constant weight, wherein the mass ratio of the sodium alginate, the deionized water and the mixed solution a was 4.6:96:20, and the mass ratio of the octenyl succinic anhydride and the isopropyl alcohol in the mixed solution a was 1.2:60; Step A2, at room temperature, the 0.8% gelatin aqueous solution and the modified sodium alginate aqueous solution were added into anhydrous ethanol, stirred at 520 rpm for 14 min until uniform, the Chinese medicine extract and zinc lactate prepared in Comparative Preparation Example 1 were added while stirring, the temperature was raised to 62℃, the stirring speed was adjusted to 1100 rpm, and the emulsification reaction was continued for 12 min, the pH was adjusted to 4.2 with 0.6% acetic acid aqueous solution, the temperature was lowered to 6℃, the pH was adjusted to 8.8 with 2.0% sodium carbonate aqueous solution, and then it was left to stand, separated, centrifuged, and dried at 54℃ until constant weight to obtain the functional ingredient, wherein the mass ratio of the gelatin aqueous solution, the modified sodium alginate aqueous solution, the anhydrous ethanol, the Chinese medicine extract and the zinc lactate was 3:1.2:50:3.6:0.6.

[0036] Comparative Preparation Example 5 The present comparative preparation example provides a functional ingredient, which is prepared by the following steps: Step A1, sodium alginate and deionized water were mixed, stirred at room temperature for 12 min at 460 rpm to uniform, adjusted to pH 8 with 5% sodium carbonate solution, then added dropwise mixed liquid a of anhydrous citric acid and isopropanol, controlled in 10 min, after dripping, heated to 68℃, stirred for 4h, then adjusted to pH 6.4 with 1% citric acid solution, washed with anhydrous ethanol and deionized water for 3 times respectively, dried at 56℃ to constant weight, to obtain modified sodium alginate, wherein the mass ratio of sodium alginate, deionized water and mixed liquid a is 4.6:96:20, in the mixed liquid a, the mass ratio of anhydrous citric acid and isopropanol is 1.2:60; Step A2, at room temperature, 0.8% gelatin aqueous solution and 4.6% modified sodium alginate aqueous solution were added into anhydrous ethanol, stirred for 14 min at 520 rpm to uniform, then prepared extract of traditional Chinese medicine and zinc lactate prepared in preparation example 1 were added while stirring, heated to 62℃, adjusted the stirring speed to 1100 rpm, continued to emulsify for 12 min, adjusted to pH 4.2 with 0.6% acetic acid solution, cooled to 6℃, then adjusted to pH 8.8 with 2.0% sodium carbonate solution, stood, separated, centrifuged, dried at 54℃ to constant weight, to obtain functional ingredients, wherein the mass ratio of gelatin aqueous solution, modified sodium alginate aqueous solution, anhydrous ethanol, traditional Chinese medicine extract and zinc lactate is 3:1.2:50:3.6:0.6.

[0037] Comparative preparation example 6 The present comparative preparation example provides a kind of functional ingredients, which is prepared by the following steps: Step A1, sodium alginate and deionized water were mixed, stirred at room temperature for 12 min at 460 rpm to uniform, adjusted to pH 8 with 5% sodium carbonate solution, then added dropwise mixed liquid a of octenyl succinic anhydride and isopropanol, controlled in 10 min, after dripping, heated to 68℃, stirred for 4h, then adjusted to pH 6.4 with 1% citric acid solution, washed with anhydrous ethanol and deionized water for 3 times respectively, dried at 56℃ to constant weight, to obtain modified sodium alginate, wherein the mass ratio of sodium alginate, deionized water and mixed liquid a is 4.6:96:20, in the mixed liquid a, the mass ratio of octenyl succinic anhydride and isopropanol is 1.2:60; Step A2, at room temperature, the 0.8% by mass gelatin aqueous solution and the 4.6% by mass modified sodium alginate aqueous solution were added into anhydrous ethanol, stirred for 14 min at a rotation speed of 520 rpm until uniform, while stirring, the extract of traditional Chinese medicine prepared in Preparation Example 1 and deionized water were added, the temperature was raised to 62℃, the rotation speed was adjusted to 1100 rpm, and the emulsification reaction was continued for 12 min, the pH was adjusted to 4.2 with 0.6% by mass acetic acid aqueous solution, the temperature was lowered to 6℃, the pH was adjusted to 8.8 with 2.0% by mass sodium carbonate aqueous solution, and then the mixture was allowed to stand, the layers were separated, centrifuged, and dried at 54℃ until the weight was constant to obtain the active ingredient, wherein the mass ratio of the gelatin aqueous solution, the modified sodium alginate aqueous solution, the anhydrous ethanol, the extract of traditional Chinese medicine, and the deionized water was 3:1.2:50:3.6:0.6.

[0038] Preparation Examples 7-9 and Comparative Preparation Examples 7-8 provide a sustained-release synergist.

[0039] Preparation Example 7 The present preparation example provides a sustained-release synergist prepared by the following steps: The anthocyanins, bromelain, and rhamnolipid were added to the phosphate buffer, the temperature was raised to 46℃, and the mixture was stirred at a rotation speed of 600 rpm for 14 min to obtain the sustained-release synergist, wherein the mass ratio of the anthocyanins, the bromelain, the rhamnolipid, and the phosphate buffer was 0.8:0.2:0.04:40.

[0040] Preparation Example 8 The present preparation example provides a sustained-release synergist prepared by the following steps: The anthocyanins, bromelain, and rhamnolipid were added to the phosphate buffer, the temperature was raised to 49℃, and the mixture was stirred at a rotation speed of 620 rpm for 16 min to obtain the sustained-release synergist, wherein the mass ratio of the anthocyanins, the bromelain, the rhamnolipid, and the phosphate buffer was 1.0:0.3:0.05:45.

[0041] Preparation Example 9 The present preparation example provides a sustained-release synergist prepared by the following steps: The anthocyanins, bromelain, and rhamnolipid were added to the phosphate buffer, the temperature was raised to 452℃, and the mixture was stirred at a rotation speed of 640 rpm for 18 min to obtain the sustained-release synergist, wherein the mass ratio of the anthocyanins, the bromelain, the rhamnolipid, and the phosphate buffer was 1.2:0.4:0.06:50.

[0042] Comparative Preparation Example 7 The present comparative preparation example provides a sustained-release synergist prepared by the following steps: Anthocyanidin and rhamnolipid are added to phosphate buffer, the temperature is raised to 46° C., and the stirring speed is controlled at 600 rpm for 14 minutes to obtain a sustained-release enhancer, wherein the mass ratio of anthocyanidin, rhamnolipid and phosphate buffer is 1:0.04:40.

[0043] Comparative Preparation Example 8 This comparative preparation example provides a sustained-release synergist prepared by the following steps: Bromelain and rhamnolipid were added to phosphate buffer, the temperature was raised to 46°C, and the mixture was stirred at a speed of 600 rpm for 14 minutes to obtain a sustained-release enhancer, wherein the mass ratio of bromelain, rhamnolipid and phosphate buffer was 1:0.04:40.

[0044] Examples 1-3 and Comparative Examples 1-6 provide a Chinese herbal toothpaste formula and a preparation method thereof.

[0045] Example 1 This embodiment provides a Chinese herbal toothpaste formula, comprising the following raw materials in parts by weight: 7 parts of the active ingredient prepared in Preparation Example 4, 2.4 parts of the sustained-release enhancer prepared in Preparation Example 7, 20 parts of nanohydroxyapatite, 28 parts of glycerin, 2.6 parts of sodium laureth sulfate, 0.16 parts of paraben, 1.8 parts of xanthan gum, 1.4 parts of peppermint, 5.8 parts of D-sorbitol, and 16 parts of deionized water; The preparation method of the Chinese herbal toothpaste comprises the following steps: Xanthan gum, glycerin, D-sorbitol and deionized water were mixed and stirred at a speed of 460 rpm for 16 minutes until uniform. Nanohydroxyapatite and sodium lauryl polyether sulfate were added. The vacuum degree was 11 Pa, and the speed was maintained unchanged. Stirring was continued for 11 minutes until uniform. Then, functional ingredients, sustained-release enhancers, peppermint and paraben were added. The speed was adjusted to 1000 rpm and stirring was continued for 6 minutes until uniform. The vacuum degree was maintained at -0.094 MPa. The mixture was bubbling for 6 minutes, discharged, and filled to obtain the Chinese herbal toothpaste.

[0046] Example 2 This embodiment provides a Chinese herbal toothpaste formula, comprising the following raw materials in parts by weight: 17.5 parts of the active ingredient prepared in Preparation Example 5, 2.6 parts of the sustained-release enhancer prepared in Preparation Example 8, 21 parts of calcium hydrogen phosphate, 30 parts of propylene glycol, 3 parts of cocamidopropyl betaine, 0.17 parts of sodium benzoate, 1.9 parts of carrageenan, 1.5 parts of spearmint, 6 parts of xylitol, and 17 parts of deionized water; The preparation method of the Chinese herbal toothpaste comprises the following steps: Mix carrageenan, propylene glycol, xylitol and deionized water, stir at 480 rpm for 18 min until uniform, add calcium hydrogen phosphate and cocamidopropyl betaine, maintain the stirring speed unchanged under vacuum degree of 12 Pa, continue to stir for 13 min until uniform, then add the efficacy ingredient, the sustained-release synergist, spearmint and sodium benzoate, adjust the stirring speed to 1100 rpm, continue to stir for 7 min until uniform, keep the vacuum degree at -0.096 MPa, defoam for 8 min, discharge, fill, to get the Chinese herbal toothpaste.

[0047] Example 3 The present example provides a Chinese herbal toothpaste formula, comprising the following raw materials by weight: 18 parts of the efficacy ingredient prepared in Preparation Example 6, 2.8 parts of the sustained-release synergist prepared in Preparation Example 9, 22 parts of nano-hydroxyapatite, 32 parts of glycerol, 3.4 parts of sodium laureth sulfate, 0.18 parts of nipagin, 2 parts of xanthan gum, 1.6 parts of peppermint, 6.2 parts of D-sorbitol and 18 parts of deionized water. The preparation method of the Chinese herbal toothpaste comprises the following steps: Mix xanthan gum, glycerol, D-sorbitol and deionized water, stir at 500 rpm for 20 min until uniform, add nano-hydroxyapatite and sodium laureth sulfate, maintain the stirring speed unchanged under vacuum degree of 13 Pa, continue to stir for 15 min until uniform, then add the efficacy ingredient, the sustained-release synergist, peppermint and nipagin, adjust the stirring speed to 1200 rpm, continue to stir for 8 min until uniform, keep the vacuum degree at -0.098 MPa, defoam for 10 min, discharge, fill, to get the Chinese herbal toothpaste.

[0048] Comparative Example 1 Comparative Example 1 is the same as Example 1, except that the efficacy ingredient in Example 1 is replaced by the efficacy ingredient prepared in Comparative Preparation Example 3.

[0049] Comparative Example 2 Comparative Example 2 is the same as Example 1, except that the efficacy ingredient in Example 1 is replaced by the efficacy ingredient prepared in Comparative Preparation Example 4.

[0050] Comparative Example 3 Comparative Example 3 is the same as Example 1, except that the efficacy ingredient in Example 1 is replaced by the efficacy ingredient prepared in Comparative Preparation Example 5.

[0051] Comparative Example 4 Comparative Example 4 is the same as Example 1, except that the efficacy ingredient in Example 1 is replaced by the efficacy ingredient prepared in Comparative Preparation Example 6.

[0052] Comparative Example 5 Comparative Example 5 is the same as Example 1, except that the sustained-release synergist in Example 1 is replaced by the sustained-release synergist prepared in Comparative Preparation Example 7.

[0053] Comparative Example 6 Comparative Example 6 is the same as Example 1, except that the sustained-release synergist in Example 1 is replaced by the sustained-release synergist prepared in Comparative Preparation Example 8.

[0054] Performance test 1. Safety test The toothpaste bodies prepared in Examples 1-3 and Comparative Examples 1-6 are uniform, free of foreign matter, do not overflow the tube opening after being filled into the tube, do not separate out liquid, have normal fragrance color, meet the standards of GB / T 8372-2017, have arsenic content far below the upper limit specified by the arsenic spot method of GB7917.2-1987, and have bacterial flora meeting the relevant provisions of the Cosmetics Safety Technical Specifications, and are all qualified.

[0055] 2. Anti-inflammatory test The experimental animals are ICR mice weighing 18-22 g provided by Shanghai Slake Experimental Animal Co., Ltd. (SCXK(Shanghai) 2017-0005). The mice are adaptively fed for one week under the conditions of 18-22℃, relative humidity of 60%-70%, and light and dark alternation for 12h / 12h.

[0056] Test basis: GQT / ZY-DL-002 “Mouse Ear Swelling Test” The 132 qualified mice are randomly divided into 11 groups, which are set as a model control group, an anti-inflammatory control group, Example 1-3 groups, and Comparative Example 1-6 groups, each group having 12 mice. The left ears of the mice in each group are not treated as the background value, and 30 μL of a dimethylbenzene solution is applied to the inner and outer surfaces of the right ears. After 30 min, except for the model control group, the mice in the Example 1-3 groups and the Comparative Example 1-6 groups have 0.1 g of the toothpaste prepared in each group applied to the right ear surfaces, and the mice in the anti-inflammatory control group have 0.1 g of the toothpaste containing forsythia suspensa and honeysuckle (containing forsythia suspensa) applied to the right ear surfaces. After 1 h of sample application, the same parts of the double ears are weighed and recorded, and the weight difference between the left and right ears is the degree of swelling, as shown in Table 1 below. Table 1 Inhibition effect of mouse ear swelling (n=11, ±s, %) As can be seen from the above, the toothpaste prepared in the Example 1-3 groups has a significantly lower degree of swelling of the mouse ears after the effect than the model control group and the Comparative Example 1-6 group, which indicates that the toothpaste formula prepared in the present application has a more excellent anti-inflammatory effect.

[0057] 3. Deodorization and stain removal test 3.1 Culture of inoculated bacterial solution P. gingivalis, P. intermedius and F. nucleatum were inoculated into nutrient broth medium and cultured under anaerobic conditions at 37°C for 2-5 days. Single colonies on the plate were picked and suspended in sterile PBS (50 mmol / L, pH 7.4) to prepare a 5 mL bacterial suspension. The suspension was adjusted to a 0.5 McFarland turbidity concentration (i.e. 1 x 10 8 CFU / mL) and then carboxymethyl cellulose was added. The mixture was filtered through a filter membrane with a pore size of 0.22 μm to prepare a bacterial inoculum containing 2% carboxymethyl cellulose.

[0058] 3.2 Establishment of an animal model of halitosis A total of 66 SPF Wistar rats, male, weighing 200 ± 20 g, were selected. The rats were healthy, active, had bright hair, good appetite, no caries and no periodontal disease. The bacterial inoculum (3 x 10 6 CFU / mL) obtained by culture was applied to the gingiva of the rats once a day for 4 weeks. The halitosis index, gingival index and plaque index of the rats were detected every week.

[0059] 3.3 Grouping of animal experiments The 66 qualified rats after successful modeling of oral application of the bacteria that easily cause halitosis were randomly divided into 11 groups, i.e. a model control group, a positive control group, Example 1-3 groups and Comparative Example 1-6 groups, 6 rats in each group. Except for the model control group, the rats in the Example 1-3 groups and Comparative Example 1-6 groups were treated with the prepared Chinese herbal toothpaste, 0.2 g per rat, once a day for 4 weeks. The rats in the positive control group were treated with the Youshijingyinhua toothpaste (containing forsythia), 0.2 g per rat, once a day for 4 weeks.

[0060] Observation indexes and detection methods The halitosis index was detected by a specially trained person according to the smell intensity of the odor sample by nose smelling method every week, and the specific detection and scoring standards were as follows: the severity was scored according to 0-5 points, 0 points, no halitosis: the examiner could not detect any odor; 1 point, barely detectable halitosis: only when the examiner deliberately smelled, could a slight odor be barely detected; 2 points, mild halitosis: the examiner could detect the odor without deliberately smelling, but the odor was weak and not strong; 3 points, moderate halitosis: the odor was obvious, the examiner could easily detect it, and the odor was uncomfortable; 4 points, severe halitosis: the odor was strong, the examiner could detect it even when he was not close to the subject's mouth, and the odor was offensive; 5 points, severe halitosis: the odor was extremely strong, the examiner could detect it obviously at a certain distance, and the odor was unbearable; the plaque index and gingival index were detected, and the specific detection and scoring standards of the plaque index were as follows: the mesio-buccal, buccal, disto-buccal and lingual surfaces of each tooth were checked at 4 points, respectively, and the sum of the 4 scores was divided by 4, which was the score of the tooth. 0 indicates no plaque in the near-gingival area; 1 indicates thin plaque in the near-gingival area, which is invisible to the naked eye and can be scraped off with the side of the probe tip; 2 indicates moderate amount of plaque on the gingival margin or adjacent surface; 3 indicates a large amount of soft dirt in the gingival sulcus or on the gingival margin and adjacent surface; the specific detection and scoring standards of the gingival index were as follows: the CPI periodontal probe recommended by WHO was used to check the mesio-buccal, buccal, disto-buccal and lingual surfaces of each tooth at 4 points, respectively, and the sum of the 4 scores was divided by 4, which was the score of the tooth. 0 indicates healthy gums; 1 indicates mild inflammation of the gums: the gum color has a slight change and has a slight edema, and the probe does not bleed; 2 indicates moderate inflammation of the gums: the gum color is red, the edema is shiny, and the probe bleeds; 3 indicates severe inflammation of the gums: the gums are obviously red and swollen or have ulcers, and have a tendency to bleed automatically. The average value is defined as mild inflammation (0-1), moderate inflammation (1-2), and severe inflammation (2-3). The specific scoring standards of the gingival index are as follows: the severity of the gingival index is scored according to 0-3 points, and the gingiva is healthy without inflammatory manifestations. 0 points, mild inflammation: the gum color changes slightly (such as darkening), and the gum is slightly edematous, and the probe does not bleed 1 point, moderate inflammation: the gum color is red, the edema is shiny, and the probe bleeds 2 points, severe inflammation: the gums are obviously red and swollen, may have ulcers, and have a tendency to bleed automatically 3 points, and the results are shown in Table 2. Table 2 Comparison of deodorization and stain removal scores of each group of rats (n=11, ±s,% Note: *: mean ± standard deviation From Table 2 above, it can be seen that the halitosis index, plaque index and gingival index of the experimental groups of rats after the action of the toothpaste prepared in Examples 1-3 were significantly lower than those of the model control group and Comparative Examples 1-6, which indicated that the Chinese herbal toothpaste prepared in the present application had more excellent effects of removing halitosis, removing stains and whitening, and stopping bleeding.

[0061] The embodiments are only illustrative of the present application, and are not intended to limit the present application, and those skilled in the art can make modifications to the embodiments without creative contribution after reading the specification, but as long as the modifications are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A Chinese herbal toothpaste formula, characterized in that: Including raw materials in parts by weight: 17-18 parts of active ingredients, 2.4-2.8 parts of sustained-release enhancers, 20-22 parts of abrasives, 28-32 parts of moisturizers, 2.6-3.4 parts of surfactants, 0.16-0.18 parts of preservatives, 1.8-2 parts of thickeners, 1.4-1.6 parts of flavors, 5.8-6.2 parts of flavorings, and 16-18 parts of deionized water; The active ingredient is firstly prepared by a ring-opening esterification reaction between sodium alginate and octenylsuccinic anhydride to obtain modified sodium alginate, and then by a complex coacervation method using gelatin and modified sodium alginate as wall materials, and traditional Chinese medicine extracts and zinc lactate as core materials; The traditional Chinese medicine extract is prepared by reflux extraction of mistletoe, thistle, plantain, sedge and forsythia.

2. A Chinese herbal toothpaste formula according to claim 1, characterized in that: The functional ingredients are prepared by the following steps: Step A1: Sodium alginate and deionized water were mixed and stirred at room temperature, and the pH value was adjusted to 8-9. A mixture of octenylsuccinic anhydride and isopropyl alcohol (a) was then added dropwise. After the addition was complete, the mixture was heated to 68-72° C. and stirred for 4-6 hours. The pH value was then adjusted to 6.4-6.8, washed, and dried to obtain modified sodium alginate. Step A2: Add the gelatin aqueous solution and the modified sodium alginate aqueous solution to anhydrous ethanol at room temperature, stir evenly, add the traditional Chinese medicine extract and zinc lactate while stirring, raise the temperature to 62-66° C., emulsify for 12-16 minutes, adjust the pH to 4.2-4.4, cool to 6-10° C., and then adjust the pH to 8.8-9.

2. Let stand, separate, centrifuge, and dry to obtain the active ingredient.

3. A Chinese herbal toothpaste formula according to claim 2, characterized in that: In step A1, the mass ratio of sodium alginate, deionized water, and mixed solution a is 4.6-5.4:96-108:20, and in the mixed solution a, the mass ratio of octenylsuccinic anhydride and isopropyl alcohol is 1.2-2.2:

60.

4. A Chinese herbal toothpaste formula according to claim 2, characterized in that: In step A2, the mass ratio of the gelatin aqueous solution, the modified sodium alginate aqueous solution, the anhydrous ethanol, the traditional Chinese medicine extract and the zinc lactate is 3-5:1.2-1.6:50-60:3.6-5.4:0.6-0.

8.

5. A Chinese herbal toothpaste formula according to claim 1, characterized in that: The Chinese medicine extract is prepared by the following steps: Step B1: Grind together the herb, thistle, plantain, sedge and forsythia, pass through a 60-100 mesh sieve, soak in deionized water for 3-5 hours, add anhydrous ethanol, reflux and extract 1-3 times, filter while hot, and collect the filtrate; Step B2, concentrating the filtrate in step B1 under reduced pressure until the anhydrous ethanol is completely evaporated, and collecting the concentrate; Step B3: dilute the concentrate from step B2 with deionized water, let it stand for 4-6 hours, centrifuge and collect the supernatant, concentrate to a thick paste with a relative density of 1.2-1.3 at 80°C, dry at 60-70°C, and crush into 120-160 mesh to obtain a Chinese medicine extract.

6. A Chinese herbal toothpaste formula according to claim 5, characterized in that: In the step B1, the mass ratio of mistletoe, thistle, plantain, sedge, forsythia, deionized water and anhydrous ethanol is 4.2-5.6:2.8-3.4:3.6-4.4:3.2-3.6:2.2-2.4:160-220:120-150.

7. A Chinese herbal toothpaste formula according to claim 5, characterized in that: In step B3, the mass ratio of the concentrate to deionized water is 1:4-5.

8. A Chinese herbal toothpaste formula according to claim 1, characterized in that: The sustained-release synergist is prepared by the following steps: Anthocyanidin, bromelain and rhamnolipid are added to phosphate buffer, heated to 46-52° C., and stirred for 14-18 minutes to obtain a sustained-release enhancer.

9. A Chinese herbal toothpaste formula according to claim 8, characterized in that: The mass ratio of anthocyanidin, bromelain, rhamnolipid and phosphate buffer is 0.8-1.2:0.2-0.4:0.04-0.06:40-50.

10. A method for preparing the Chinese herbal toothpaste formula according to any one of claims 1 to 9, characterized in that: The following steps are involved: Mix the thickener, moisturizer, flavoring and deionized water, stir evenly, add the abrasive and surfactant and stir evenly in vacuum, then add the functional ingredients, sustained-release enhancer, flavor and preservative and continue to stir evenly, maintain vacuum, bubbling for 6-10 minutes, discharge the material, and fill it to obtain the Chinese herbal toothpaste.

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