CN115068386A - Toothpaste containing calendula officinalis mixed extract and preparation method thereof - Google Patents

Abstract

The invention is suitable for the technical field of toothpaste, and provides toothpaste containing calendula officinalis mixed extract and a preparation method thereof, wherein the toothpaste comprises the following raw materials: the toothpaste containing the calendula mixed extract has the effects of promoting blood circulation, stopping bleeding, resisting bacteria, diminishing inflammation and treating dental ulcer by adding the calendula extract, has certain antibacterial effect on staphylococcus and streptococcus in an oral cavity, has the effects of clearing heat, removing toxicity, cooling blood and stopping bleeding by adding the honeysuckle extract, has the effects of resisting bacteria, resisting viruses, clearing heat, diminishing inflammation and resisting oxidation and preventing gingival atrophy by squeezing the chrysanthemum extract, and has better single compatibility effect in the toothpaste and better synergistic effect compared with the toothpaste prepared by compounding the calendula, the honeysuckle extract and the chrysanthemum extract.

Description

Toothpaste containing calendula officinalis mixed extract and preparation method thereof

Technical Field

The invention belongs to the technical field of toothpaste, and particularly relates to toothpaste containing calendula officinalis mixed extract and a preparation method thereof.

Background

The pathological phenomena of the oral cavity under the conditions of damage of external physicochemical factors, invasion of pathogens, abnormal development of the dentognathic and maxillofacial surfaces, systemic diseases and the like are various, and the diseases are originally generated in the oral cavity;

common oral diseases such as periodontal diseases, oral ulcers and the like are mainly caused by pathogenic bacteria existing in the oral cavity, the existing method for treating the oral ulcers comprises the steps of directly spraying anti-inflammatory and bactericidal powder on an affected part, orally taking an anti-inflammatory drug for diminishing inflammation for serious patients, causing no serious pain during spraying, being difficult to accept by many people, having slow drug effect of the anti-inflammatory drug, and injuring intestines and stomach, and is not the optimal choice;

the toothpaste is one of tooth cleaning products, is generally in a gel shape, is usually smeared on a toothbrush, cleans the surfaces of teeth by the mechanical friction action of the toothbrush, cleans the teeth and the periphery of the teeth and purifies and refreshes the oral cavity; some existing toothpaste also has a certain prevention and treatment effect on oral ulcer, but the effect is not obvious and the cure period is long.

Disclosure of Invention

The invention provides toothpaste containing calendula mixing extract and a preparation method thereof, and aims to solve the problems that some existing toothpaste has certain prevention and treatment effects on dental ulcer, but the effect is not obvious and the cure period is long.

The invention is realized in such a way that the toothpaste containing the calendula officinalis mixed extract comprises the following raw materials in parts by weight: 5-15 parts of a traditional Chinese medicine extract, 400 parts of a humectant, 300 parts of an abrasive, 5-10 parts of a preservative, 10-15 parts of an aromatic, 8-20 parts of a thickening agent, 1-3 parts of a sugar flavor agent and 300 parts of deionized water, wherein the traditional Chinese medicine extract is prepared from a calendula extract, a honeysuckle extract and a chrysanthemum extract according to a mass ratio of 1-5:1: 1.

Preferably, the toothpaste containing the calendula officinalis mixed extract comprises the following raw materials in parts by weight: 8-12 parts of traditional Chinese medicine extract, 350 parts of humectant 200-.

Preferably, the toothpaste containing the calendula officinalis mixed extract comprises the following raw materials in parts by weight: the traditional Chinese medicine composition comprises 10 parts of traditional Chinese medicine extract, 275 parts of humectant, 250 parts of abrasive, 8 parts of preservative, 13 parts of aromatic, 14 parts of thickening agent, 2 parts of sugar flavor agent and 225 parts of deionized water, wherein the traditional Chinese medicine extract is compounded by calendula extract, honeysuckle extract and chrysanthemum extract according to the mass ratio of 3:1: 1.

Preferably, the calendula extract is prepared by the following method: extracting calendula officinalis with ethanol to obtain a dilute extract; extracting the thin extract by an organic solvent, collecting extract liquor, recovering the organic solvent under reduced pressure, and drying to obtain an extract; dissolving the extract with ethanol, adsorbing with resin, eluting with ethanol to remove impurities, and gradient eluting with ethanol to obtain calendula extract adsorbed on resin; collecting eluate, concentrating under reduced pressure, drying, and pulverizing to obtain herba Sidae Rhombifoliae extract.

Preferably, the ratio of the medicinal material weight of the calendula officinalis to the volume of the ethanol is 1:3-7 in g/mL, the organic solvent is ethyl acetate, and the volume ratio of the dilute extract to the ethyl acetate is 1: 1-3, wherein the resin is AB-8 or HPD100, the volume concentration of ethanol extracted by ethanol is 50-80%, the volume concentration of ethanol leached to remove impurities is 30-60%, and the volume concentration of ethanol eluted by gradient is 50-90%.

Preferably, the preparation method of the honeysuckle extract comprises the following steps: taking 100-180 parts by weight of honeysuckle flower, grinding, adding the ground honeysuckle flower into 180-150 parts by weight of potassium sulfate solution with the mass concentration of 0.5-1%, uniformly stirring, heating, extracting, and cooling to obtain a leaching solution; feeding the leaching solution into macroporous adsorption resin for adsorption, and collecting the permeate; adjusting the pH value of the permeate to 8-10, and filtering with an ultrafiltration membrane to obtain ultrafiltration permeate; adding 40-60 parts of ethyl acetate into the ultrafiltration permeate liquid for extraction to obtain an organic phase; heating and concentrating the organic phase, and obtaining the honeysuckle extract when the volume of the feed liquid is reduced to 10-20% of the original volume.

Preferably, the preparation method of the chrysanthemum extract comprises the following steps: adding flos Chrysanthemi into 10-16 weight times of water to obtain primary extractive solution, vacuumizing, heating to 80-100 deg.C to boil the primary extractive solution, maintaining the temperature for 1-3 hr, and filtering to obtain primary filtrate and residue; adding the filter residue into water 8-12 times the weight of the filter residue to obtain a secondary immersion liquid, vacuumizing the secondary immersion liquid, heating to 60-80 ℃ to boil the secondary immersion liquid, preserving heat for 1-3h, and filtering to obtain a secondary filtrate; mixing the primary filtrate and the secondary filtrate, and concentrating under reduced pressure to obtain extract with relative density of 1.2-1.3; and drying and crushing the extract in vacuum to obtain the chrysanthemum extract.

Preferably, the humectant is a mixture of glycerin and sorbitol, the abrasive is one or more of calcium carbonate, calcium hydrogen phosphate, calcium pyrophosphate, hydrated silicic acid and aluminum hydroxide, and the preservative is sodium benzoate.

Preferably, the aromatic is spearmint essence, the thickening agent is xanthan gum, and the sugar flavor is xylitol.

The preparation method of the toothpaste containing the calendula officinalis mixed extract comprises the following steps:

1) weighing the raw materials according to the proportion;

2) mixing herba Sidae Rhombifoliae extract, flos Lonicerae extract, flos Chrysanthemi extract and half of deionized water, stirring well, and stirring for 20-30min to obtain mixture A;

3) feeding mixture A, humectant, abrasive, antiseptic, and thickener into paste making machine, high-speed stirring and grinding for 30-40min, adding aromatic and sugar flavoring agent, stirring for 20-30min, and vacuum degassing to obtain the final product.

Compared with the prior art, the embodiment of the application mainly has the following beneficial effects:

the toothpaste containing the calendula mixed extract has the effects of activating blood circulation, stopping bleeding, resisting bacteria, diminishing inflammation and treating dental ulcer by adding the calendula extract, has a certain antibacterial effect on staphylococcus and streptococcus in an oral cavity, has the effects of clearing away heat and toxic materials, cooling blood and stopping bleeding by adding the honeysuckle extract, has the effects of resisting bacteria and viruses, clearing away heat, diminishing inflammation and resisting oxidation and preventing gingival atrophy by squeezing the chrysanthemum extract, has a better compatibility effect in the toothpaste by compounding the calendula, the honeysuckle and the chrysanthemum, and can play a good synergistic effect mutually so that the toothpaste can more effectively diminish inflammation, eliminate fire, resist bacteria, protect gum and heal the dental ulcer.

Drawings

FIG. 1 is a flow chart of the preparation of toothpaste containing calendula officinalis mixed extract provided by the present invention.

Detailed Description

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having," and any variations thereof, in the description and claims of this application are intended to cover non-exclusive inclusions. The terms first, second and the like in the description and in the claims of the present application are used for distinguishing between different objects and not for describing a particular sequential order.

Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.

Example 1

The embodiment of the invention prepares toothpaste containing calendula officinalis mixed extract, as shown in figure 1, the following raw materials are weighed according to the proportion by weight: the traditional Chinese medicine composition comprises, by mass, 5 parts of a traditional Chinese medicine extract, 150 parts of a humectant, 200 parts of an abrasive, 5 parts of a preservative, 10 parts of an aromatic, 8 parts of a thickening agent, 1 part of a sugar flavor and 150 parts of deionized water, wherein the traditional Chinese medicine extract is prepared by compounding a calendula extract, a honeysuckle extract and a chrysanthemum extract according to a mass ratio of 1:1:1, and the calendula extract, the honeysuckle extract, the chrysanthemum extract and half of the deionized water are mixed and stirred uniformly for 20min to obtain a mixture A; feeding mixture A, humectant, abrasive, antiseptic, and thickener into paste making machine, high-speed stirring and grinding for 30min, adding aromatic and sugar flavoring agent, stirring for 20min, and vacuum degassing to obtain the final product.

The preparation method of the calendula extract comprises the following steps: extracting calendula officinalis with ethanol to obtain a dilute extract; extracting the thin extract by an organic solvent, collecting extract liquor, recovering the organic solvent under reduced pressure, and drying to obtain an extract; dissolving the extract with ethanol, adsorbing with resin, eluting with ethanol to remove impurities, and gradient eluting with ethanol to obtain calendula extract adsorbed on resin; collecting eluate, concentrating under reduced pressure, drying, and pulverizing to obtain herba Sidae Rhombifoliae extract.

Further, the ratio of the weight of the medicinal materials of the calendula officinalis to the volume of the ethanol is 1:3 in g/mL, the organic solvent is ethyl acetate, and the volume ratio of the dilute extract to the ethyl acetate is 1:1, the resin is HPD100, the volume concentration of ethanol extracted by ethanol is 50%, the volume concentration of ethanol leached to remove impurities is 30%, and the volume concentration of ethanol eluted by gradient is 50%.

Specifically, the preparation method of the honeysuckle extract comprises the following steps: taking 100 parts by weight of honeysuckle, grinding, adding the ground honeysuckle into 150 parts by weight of potassium sulfate solution with the mass concentration of 0.5%, uniformly stirring, heating, extracting, and cooling to obtain leaching liquor; feeding the leaching solution into macroporous adsorption resin for adsorption, and collecting the permeate; adjusting the pH value of the permeate to 8, and filtering with an ultrafiltration membrane to obtain ultrafiltration permeate; adding 40 parts of ethyl acetate into the ultrafiltration permeating liquid for extraction to obtain an organic phase; heating and concentrating the organic phase, and obtaining the honeysuckle extract when the volume of the feed liquid is reduced to 10% of the original volume.

Furthermore, the preparation method of the chrysanthemum extract comprises the following steps: adding chrysanthemum into water of which the weight is 10 times that of the chrysanthemum to obtain primary immersion liquid, vacuumizing the primary immersion liquid, heating to 80 ℃ to boil the primary immersion liquid, preserving heat for 1h, and filtering to obtain primary filtrate and filter residue; adding the filter residue into water with the weight of 8 times of that of the filter residue to obtain a secondary immersion liquid, vacuumizing the secondary immersion liquid, heating to 60 ℃ to boil the secondary immersion liquid, preserving heat for 1h, and filtering to obtain a secondary filtrate; mixing the primary filtrate and the secondary filtrate, and concentrating under reduced pressure to obtain extract with relative density of 1.2; and drying and crushing the extract in vacuum to obtain the chrysanthemum extract.

Preferably, the humectant is a mixture of glycerol and sorbitol, the abrasive is calcium carbonate, the preservative is sodium benzoate, the aromatic is spearmint essence, the thickener is xanthan gum, and the sugar flavor is xylitol.

Example 2

The embodiment of the invention prepares toothpaste containing calendula officinalis mixed extract, as shown in figure 1, the following raw materials are weighed according to the proportion by weight: 8 parts of a traditional Chinese medicine extract, 200 parts of a humectant, 220 parts of an abrasive, 6 parts of a preservative, 11 parts of an aromatic, 12 parts of a thickening agent, 1.5 parts of a sugar flavor agent and 200 parts of deionized water, wherein the traditional Chinese medicine extract is prepared by compounding a calendula extract, a honeysuckle extract and a chrysanthemum extract according to a mass ratio of 2:1:1, and the calendula extract, the honeysuckle extract, the chrysanthemum extract and half of the deionized water are mixed and stirred uniformly for 20min to obtain a mixture A; feeding mixture A, humectant, abrasive, antiseptic, and thickener into paste making machine, high-speed stirring and grinding for 30min, adding aromatic and sugar flavoring agent, stirring for 20min, and vacuum degassing to obtain the final product.

The preparation method of the calendula extract comprises the following steps: extracting calendula officinalis with ethanol to obtain a dilute extract; extracting the thin extract by an organic solvent, collecting extract liquor, recovering the organic solvent under reduced pressure, and drying to obtain an extract; dissolving the extract with ethanol, adsorbing with resin, eluting with ethanol to remove impurities, and gradient eluting with ethanol to obtain calendula extract adsorbed on resin; collecting eluate, concentrating under reduced pressure, drying, and pulverizing to obtain herba Sidae Rhombifoliae extract.

Further, the ratio of the weight of the medicinal materials of the calendula officinalis to the volume of the ethanol is 1:3 in g/mL, the organic solvent is ethyl acetate, and the volume ratio of the dilute extract to the ethyl acetate is 1:1, the resin is HPD100, the volume concentration of ethanol extracted by ethanol is 50%, the volume concentration of ethanol leached to remove impurities is 30%, and the volume concentration of ethanol eluted by gradient is 50%.

Specifically, the preparation method of the honeysuckle extract comprises the following steps: taking 100 parts by weight of honeysuckle, grinding, adding the ground honeysuckle into 150 parts by weight of potassium sulfate solution with the mass concentration of 0.5%, uniformly stirring, heating, extracting, and cooling to obtain leaching liquor; feeding the leaching solution into macroporous adsorption resin for adsorption, and collecting the permeate; adjusting the pH value of the permeate to 8, and filtering with an ultrafiltration membrane to obtain ultrafiltration permeate; adding 40 parts of ethyl acetate into the ultrafiltration permeating liquid for extraction to obtain an organic phase; heating and concentrating the organic phase, and obtaining the honeysuckle extract when the volume of the feed liquid is reduced to 10% of the original volume.

Furthermore, the preparation method of the chrysanthemum extract comprises the following steps: adding chrysanthemum into water of which the weight is 10 times that of the chrysanthemum to obtain primary immersion liquid, vacuumizing the primary immersion liquid, heating to 80 ℃ to boil the primary immersion liquid, preserving heat for 1h, and filtering to obtain primary filtrate and filter residue; adding the filter residue into water with the weight of 8 times of that of the filter residue to obtain a secondary immersion liquid, vacuumizing the secondary immersion liquid, heating to 60 ℃ to boil the secondary immersion liquid, preserving heat for 1h, and filtering to obtain a secondary filtrate; mixing the primary filtrate and the secondary filtrate, and concentrating under reduced pressure to obtain extract with relative density of 1.2; and drying and crushing the extract in vacuum to obtain the chrysanthemum extract.

Preferably, the humectant is a mixture of glycerol and sorbitol, the abrasive is calcium hydrogen phosphate, the preservative is sodium benzoate, the aromatic is spearmint essence, the thickener is xanthan gum, and the sugar flavor is xylitol.

Example 3

The embodiment of the invention prepares toothpaste containing calendula officinalis mixed extract, as shown in figure 1, the following raw materials are weighed according to the proportion by weight: 10 parts of a traditional Chinese medicine extract, 275 parts of a humectant, 250 parts of an abrasive, 8 parts of a preservative, 13 parts of an aromatic, 14 parts of a thickening agent, 2 parts of a sugar flavor agent and 225 parts of deionized water, wherein the traditional Chinese medicine extract is prepared by compounding a calendula extract, a honeysuckle extract and a chrysanthemum extract according to a mass ratio of 3:1:1, and the calendula extract, the honeysuckle extract, the chrysanthemum extract and half of the deionized water are mixed and stirred uniformly for 25min to obtain a mixture A; feeding mixture A, humectant, abrasive, antiseptic, and thickener into paste making machine, high-speed stirring and grinding for 35min, adding aromatic and sugar flavoring agent, stirring for 25min, and vacuum degassing to obtain the final product.

The preparation method of the calendula extract comprises the following steps: extracting calendula officinalis with ethanol to obtain a dilute extract; extracting the thin extract by an organic solvent, collecting extract liquor, recovering the organic solvent under reduced pressure, and drying to obtain an extract; dissolving the extract with ethanol, adsorbing with resin, eluting with ethanol to remove impurities, and gradient eluting with ethanol to obtain calendula extract adsorbed on resin; collecting eluate, concentrating under reduced pressure, drying, and pulverizing to obtain herba Sidae Rhombifoliae extract.

Further, the ratio of the weight of the medicinal materials of the calendula officinalis to the volume of the ethanol is 1:5 in g/mL, the organic solvent is ethyl acetate, and the volume ratio of the dilute extract to the ethyl acetate is 1: 2, the resin is AB-8, the volume concentration of ethanol extracted by ethanol is 65%, the volume concentration of ethanol subjected to impurity removal by leaching is 45%, and the volume concentration of ethanol subjected to gradient elution is 70%.

Specifically, the preparation method of the honeysuckle extract comprises the following steps: taking 110 parts by weight of honeysuckle, grinding, adding the ground honeysuckle into 165 parts by weight of potassium sulfate solution with the mass concentration of 0.75%, uniformly stirring, heating, extracting, and cooling to obtain leaching liquor; feeding the leaching solution into macroporous adsorption resin for adsorption, and collecting the permeate; adjusting the pH value of the permeate to 9, and filtering with an ultrafiltration membrane to obtain ultrafiltration permeate; adding 50 parts of ethyl acetate into the ultrafiltration permeate to extract to obtain an organic phase; heating and concentrating the organic phase, and obtaining the honeysuckle extract when the volume of the feed liquid is reduced to 15% of the original volume.

Furthermore, the preparation method of the chrysanthemum extract comprises the following steps: adding chrysanthemum into water 13 times the weight of the chrysanthemum to obtain primary extract, vacuumizing the primary extract, heating to 90 ℃ to boil the primary extract, preserving heat for 2 hours, and filtering to obtain primary filtrate and filter residue; adding the filter residue into water with the weight of 10 times of the filter residue to obtain a secondary immersion liquid, vacuumizing the secondary immersion liquid, heating to 70 ℃ to boil the secondary immersion liquid, preserving heat for 2 hours, and filtering to obtain a secondary filtrate; mixing the primary filtrate and the secondary filtrate, and concentrating under reduced pressure to obtain extract with relative density of 1.25; and drying and crushing the extract in vacuum to obtain the chrysanthemum extract.

Preferably, the humectant is a mixture of glycerol and sorbitol, the abrasive is a mixture of calcium carbonate, calcium hydrogen phosphate, calcium pyrophosphate and the like in a mass ratio, the preservative is sodium benzoate, the aromatic is spearmint essence, the thickening agent is xanthan gum, and the sugar flavor agent is xylitol.

Example 4

The embodiment of the invention prepares toothpaste containing calendula officinalis mixed extract, as shown in figure 1, and the following raw materials are weighed according to the mixture ratio in parts by weight: 12 parts of a traditional Chinese medicine extract, 350 parts of a humectant, 280 parts of an abrasive, 9 parts of a preservative, 14 parts of an aromatic, 16 parts of a thickening agent, 1.2.5 parts of a sugar flavor agent and 250 parts of deionized water, wherein the traditional Chinese medicine extract is prepared by compounding a calendula extract, a honeysuckle extract and a chrysanthemum extract according to a mass ratio of 4:1:1, mixing and stirring the calendula extract, the honeysuckle extract, the chrysanthemum extract and half of the deionized water uniformly, and stirring for 30min to obtain a mixture A; feeding mixture A, humectant, abrasive, antiseptic, and thickener into paste making machine, high-speed stirring and grinding for 40min, adding aromatic and sugar flavoring agent, stirring for 30min, and vacuum degassing to obtain the final product.

The preparation method of the calendula extract comprises the following steps: extracting calendula officinalis with ethanol to obtain a dilute extract; extracting the thin extract by an organic solvent, collecting extract liquor, recovering the organic solvent under reduced pressure, and drying to obtain an extract; dissolving the extract with ethanol, adsorbing with resin, eluting with ethanol to remove impurities, and gradient eluting with ethanol to obtain herba Sidae Rhombifoliae extract adsorbed on resin; collecting eluate, concentrating under reduced pressure, drying, and pulverizing to obtain herba Sidae Rhombifoliae extract.

Further, the ratio of the weight of the medicinal materials of the calendula officinalis to the volume of the ethanol is 1:7 in g/mL, the organic solvent is ethyl acetate, and the volume ratio of the dilute extract to the ethyl acetate is 1: and 3, the resin is AB-8, the volume concentration of ethanol extracted by ethanol is 80%, the volume concentration of ethanol subjected to leaching to remove impurities is 60%, and the volume concentration of ethanol subjected to gradient elution is 90%.

Specifically, the preparation method of the honeysuckle extract comprises the following steps: taking 120 parts by weight of honeysuckle, grinding, adding the ground honeysuckle into 180 parts by weight of potassium sulfate solution with the mass concentration of 0.1%, uniformly stirring, heating, extracting, and cooling to obtain leaching liquor; feeding the leaching solution into macroporous adsorption resin for adsorption, and collecting the permeate; adjusting the pH value of the permeate to 10, and filtering with an ultrafiltration membrane to obtain ultrafiltration permeate; adding 60 parts of ethyl acetate into the ultrafiltration permeating liquid for extraction to obtain an organic phase; heating and concentrating the organic phase, and obtaining the honeysuckle extract when the volume of the feed liquid is reduced to 20% of the original volume.

Furthermore, the preparation method of the chrysanthemum extract comprises the following steps: adding chrysanthemum into water 16 times the weight of the chrysanthemum to obtain primary immersion liquid, vacuumizing the primary immersion liquid, heating to 100 ℃ to boil the primary immersion liquid, preserving heat for 3 hours, and filtering to obtain primary filtrate and filter residue; adding the filter residue into water with the weight of 12 times of the filter residue to obtain a secondary immersion liquid, vacuumizing the secondary immersion liquid, heating to 80 ℃ to boil the secondary immersion liquid, preserving heat for 3 hours, and filtering to obtain a secondary filtrate; mixing the primary filtrate and the secondary filtrate, and concentrating under reduced pressure to obtain extract with relative density of 1.1.3; and drying and crushing the extract in vacuum to obtain the chrysanthemum extract.

Preferably, the humectant is a mixture of glycerol and sorbitol, the abrasive is hydrated silicic acid, the preservative is sodium benzoate, the aromatic is spearmint essence, the thickener is xanthan gum, and the sugar flavor is xylitol.

Example 5

The embodiment of the invention prepares toothpaste containing calendula officinalis mixed extract, as shown in figure 1, the following raw materials are weighed according to the proportion by weight: 15 parts of a traditional Chinese medicine extract, 400 parts of a humectant, 300 parts of an abrasive, 10 parts of a preservative, 15 parts of an aromatic, 20 parts of a thickening agent, 3 parts of a sugar flavor agent and 300 parts of deionized water, wherein the traditional Chinese medicine extract is prepared by compounding a calendula extract, a honeysuckle extract and a chrysanthemum extract according to a mass ratio of 5:1:1, and the calendula extract, the honeysuckle extract, the chrysanthemum extract and half of the deionized water are mixed and stirred uniformly for 30min to obtain a mixture A; feeding mixture A, humectant, abrasive, antiseptic, and thickener into paste making machine, high speed stirring and grinding for 40min, adding aromatic and sugar flavoring agent, stirring for 30min, and vacuum degassing to obtain the final product.

The preparation method of the calendula extract comprises the following steps: extracting calendula officinalis with ethanol to obtain a dilute extract; extracting the thin extract by an organic solvent, collecting extract liquor, recovering the organic solvent under reduced pressure, and drying to obtain an extract; dissolving the extract with ethanol, adsorbing with resin, eluting with ethanol to remove impurities, and gradient eluting with ethanol to obtain calendula extract adsorbed on resin; collecting eluate, concentrating under reduced pressure, drying, and pulverizing to obtain herba Sidae Rhombifoliae extract.

Further, the ratio of the weight of the medicinal materials of the calendula officinalis to the volume of the ethanol is 1:7 in g/mL, the organic solvent is ethyl acetate, and the volume ratio of the dilute extract to the ethyl acetate is 1: and 3, the resin is AB-8, the volume concentration of ethanol extracted by ethanol is 80%, the volume concentration of ethanol subjected to leaching to remove impurities is 60%, and the volume concentration of ethanol subjected to gradient elution is 90%.

Specifically, the preparation method of the honeysuckle extract comprises the following steps: taking 120 parts by weight of honeysuckle, grinding, adding the ground honeysuckle into 180 parts by weight of potassium sulfate solution with the mass concentration of 0.1%, uniformly stirring, heating, extracting, and cooling to obtain leaching liquor; feeding the leaching solution into macroporous adsorption resin for adsorption, and collecting the permeate; adjusting the pH value of the permeate to 10, and filtering with an ultrafiltration membrane to obtain ultrafiltration permeate; adding 60 parts of ethyl acetate into the ultrafiltration permeating liquid for extraction to obtain an organic phase; heating and concentrating the organic phase, and obtaining the honeysuckle extract when the volume of the feed liquid is reduced to 20% of the original volume.

Furthermore, the preparation method of the chrysanthemum extract comprises the following steps: adding chrysanthemum into water 16 times the weight of the chrysanthemum to obtain primary immersion liquid, vacuumizing the primary immersion liquid, heating to 100 ℃ to boil the primary immersion liquid, preserving heat for 3 hours, and filtering to obtain primary filtrate and filter residue; adding the filter residue into water with the weight of 12 times of the filter residue to obtain a secondary immersion liquid, vacuumizing the secondary immersion liquid, heating to 80 ℃ to boil the secondary immersion liquid, preserving heat for 3 hours, and filtering to obtain a secondary filtrate; mixing the primary filtrate and the secondary filtrate, and concentrating under reduced pressure to obtain extract with relative density of 1.1.3; and drying and crushing the extract in vacuum to obtain the chrysanthemum extract.

Preferably, the humectant is a mixture of glycerol and sorbitol, the abrasive is aluminum hydroxide, the preservative is sodium benzoate, the aromatic is spearmint essence, the thickener is xanthan gum, and the sugar flavor is xylitol.

Comparative example 1

On the basis of the embodiment 3, the traditional Chinese medicine extract is the marigold extract only;

comparative example 2

On the basis of the embodiment 3, the traditional Chinese medicine extract is only the honeysuckle extract;

comparative example 3

On the basis of the embodiment 3, the traditional Chinese medicine extract is only chrysanthemum extract;

comparative example 4

On the basis of example 3, the calendula extract, the honeysuckle extract and the chrysanthemum extract are not contained.

Comparative example 5

On the basis of the embodiment 3, the traditional Chinese medicine extract is prepared by combining a calendula extract, a honeysuckle extract and a chrysanthemum extract according to the mass ratio of 2:1: 1;

comparative example 6

On the basis of the embodiment 3, the traditional Chinese medicine extract is prepared by combining a calendula extract, a honeysuckle extract and a chrysanthemum extract according to the mass ratio of 4:1: 1.

Test of

330 patients with 20-65-year-old oral ulcer are screened from an outpatient clinic, randomly divided into 11 groups, and 30 groups respectively correspond to examples 1-5 and comparative examples 1-6, when the toothpaste is used, the toothpaste is smeared on an affected part before three meals for 10min, the affected part is gargled after 5min, and then the patients eat the toothpaste 2 times in the morning and evening, and the teeth are brushed normally. The test was carried out after 3 weeks, respectively, and the results are shown in the following table.

The evaluation standard of the curative effect is as follows:

the change is very obvious-the total ulcer number is obviously reduced, and the symptoms of swelling and aching of gum and bleeding of gum disappear;

changes, the total ulcer number is reduced, the symptoms such as gum swelling and aching and gum bleeding are reduced or the attack period is prolonged;

the change is not significant-the total ulcer number has no obvious change or symptoms such as gum swelling and pain, gum bleeding and the like have no obvious relief;

no change-no change in the total ulcer number, no reduction in symptoms such as gingival swelling and pain and gingival bleeding;

the above results clearly show that the toothpaste prepared by the method has an obvious effect on treating dental ulcer, the number of people remarkably increasing due to the combination of the three extracts of the calendula, the honeysuckle and the chrysanthemum, the change is obvious, the compatibility effect is better than that of a single toothpaste, the extracts can play a good synergistic effect, and the optimal ratio of the combination of the calendula, the honeysuckle and the chrysanthemum is 3:1: 1.

it should be noted that, for simplicity of description, the above-mentioned embodiments are described as a series of acts, but those skilled in the art will recognize that the present invention is not limited by the order of acts, as some steps may occur in other orders or concurrently in accordance with the invention. Further, those skilled in the art should also appreciate that the embodiments described in the specification are preferred embodiments and that the acts and modules referred to are not necessarily required by the invention.

The above examples are only used to illustrate the technical solutions of the present invention, and do not limit the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from these embodiments without inventive step, are within the scope of the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art may still make various combinations, additions, deletions or other modifications of the features of the embodiments of the present invention according to the situation without conflict, so as to obtain different technical solutions without substantially departing from the spirit of the present invention, and these technical solutions also fall within the protection scope of the present invention.

Claims (10)

1. The toothpaste containing the calendula officinalis mixed extract is characterized by comprising the following raw materials in parts by weight: 5-15 parts of a traditional Chinese medicine extract, 400 parts of a humectant, 300 parts of an abrasive, 5-10 parts of a preservative, 10-15 parts of an aromatic, 8-20 parts of a thickening agent, 1-3 parts of a sugar flavor agent and 300 parts of deionized water, wherein the traditional Chinese medicine extract is prepared from a calendula extract, a honeysuckle extract and a chrysanthemum extract according to a mass ratio of 1-5:1: 1.

2. The toothpaste containing calendula mixed extract as claimed in claim 1, comprising the following raw materials in parts by weight: 8-12 parts of traditional Chinese medicine extract, 350 parts of humectant 200-.

3. The toothpaste containing calendula mixed extract as claimed in claim 2, comprising the following raw materials in parts by weight: the traditional Chinese medicine composition comprises 10 parts of traditional Chinese medicine extract, 275 parts of humectant, 250 parts of abrasive, 8 parts of preservative, 13 parts of aromatic, 14 parts of thickening agent, 2 parts of sugar flavor agent and 225 parts of deionized water, wherein the traditional Chinese medicine extract is compounded by calendula extract, honeysuckle extract and chrysanthemum extract according to the mass ratio of 3:1: 1.

4. The toothpaste containing calendula mixed extract as claimed in claim 1, wherein the calendula extract is prepared by the following method: extracting calendula officinalis with ethanol to obtain a dilute extract; extracting the thin extract by an organic solvent, collecting extract liquor, recovering the organic solvent under reduced pressure, and drying to obtain an extract; dissolving the extract with ethanol, adsorbing with resin, eluting with ethanol to remove impurities, and gradient eluting with ethanol to obtain calendula extract adsorbed on resin; collecting eluate, concentrating under reduced pressure, drying, and pulverizing to obtain herba Sidae Rhombifoliae extract.

5. The toothpaste containing calendula officinalis mixed extract according to claim 4, wherein the ratio of the medicinal material weight to the volume of ethanol in g/mL is 1:3-7, the organic solvent is ethyl acetate, and the volume ratio of the dilute extract to the ethyl acetate is 1: 1-3, wherein the resin is AB-8 or HPD100, the volume concentration of ethanol extracted by ethanol is 50-80%, the volume concentration of ethanol leached to remove impurities is 30-60%, and the volume concentration of ethanol eluted by gradient is 50-90%.

6. The toothpaste containing calendula officinalis mixed extract as claimed in claim 1, wherein the honeysuckle extract is prepared by the following method: taking 100-180 parts by weight of honeysuckle flower, grinding, adding the ground honeysuckle flower into 180-150 parts by weight of potassium sulfate solution with the mass concentration of 0.5-1%, uniformly stirring, heating, extracting, and cooling to obtain a leaching solution; feeding the leaching solution into macroporous adsorption resin for adsorption, and collecting the permeate; adjusting the pH value of the permeate to 8-10, and filtering with an ultrafiltration membrane to obtain ultrafiltration permeate; adding 40-60 parts of ethyl acetate into the ultrafiltration permeate liquid for extraction to obtain an organic phase; heating and concentrating the organic phase, and obtaining the honeysuckle extract when the volume of the feed liquid is reduced to 10-20% of the original volume.

7. The toothpaste comprising calendula officinalis mixed extract according to claim 1, wherein the chrysanthemum extract is prepared by the following method: adding flos Chrysanthemi into 10-16 weight times of water to obtain primary extractive solution, vacuumizing, heating to 80-100 deg.C to boil the primary extractive solution, maintaining the temperature for 1-3 hr, and filtering to obtain primary filtrate and residue; adding the filter residue into water 8-12 times the weight of the filter residue to obtain a secondary immersion liquid, vacuumizing the secondary immersion liquid, heating to 60-80 ℃ to boil the secondary immersion liquid, preserving heat for 1-3h, and filtering to obtain a secondary filtrate; mixing the primary filtrate and the secondary filtrate, and concentrating under reduced pressure to obtain extract with relative density of 1.2-1.3; and drying and crushing the extract in vacuum to obtain the chrysanthemum extract.

8. The toothpaste containing calendula mixing extract as claimed in claim 1, wherein the humectant is a mixture of glycerin and sorbitol, the abrasive is one or more combination of calcium carbonate, calcium hydrogen phosphate, calcium pyrophosphate, hydrated silicic acid and aluminum hydroxide, and the preservative is sodium benzoate.

9. The toothpaste of claim 1, wherein said flavoring agent is spearmint flavor, said thickening agent is xanthan gum, and said sugar flavoring agent is xylitol.

10. The method for preparing calendula officinalis containing mixed extract according to any one of claims 1 to 9, wherein the calendula officinalis containing mixed extract is prepared by a method comprising the steps of:

1) weighing the raw materials according to the proportion;

2) mixing herba Sidae Rhombifoliae extract, flos Lonicerae extract, flos Chrysanthemi extract and half of deionized water, stirring well, and stirring for 20-30min to obtain mixture A;

3) feeding mixture A, humectant, abrasive, antiseptic, and thickener into paste making machine, high-speed stirring and grinding for 30-40min, adding aromatic and sugar flavoring agent, stirring for 20-30min, and vacuum degassing to obtain the final product.

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