(3) summary of the invention
The object of the present invention is to provide a kind of have heat-clearing and toxic substances removing, dispersing swelling and dissipating binds, antibacterial anti-inflammatory, antiviral effect; Can improve the gingiva relevant issues, eliminate or alleviate the SHUANGHUANLIAN Chinese medicinal toothpaste of halitosis.The present invention also aims to provide a kind of preparation method of SHUANGHUANLIAN Chinese medicinal toothpaste.
The object of the present invention is achieved like this:
Contain Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract 0.03~10g, Radix Scutellariae extract 0.03~10g, Fructus Forsythiae extract 0.03~10g among the every 100g of SHUANGHUANLIAN Chinese medicinal toothpaste of the present invention.
The preferred group of SHUANGHUANLIAN Chinese medicinal toothpaste of the present invention becomes: contain Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract 0.05~5g, Radix Scutellariae extract 0.05~5g, Fructus Forsythiae extract 0.05~5g among every 100g.
The preparation method of SHUANGHUANLIAN Chinese medicinal toothpaste of the present invention is:
Radix Scutellariae decocts with water three times, first, secondary each 2 hours, 1 hour for the third time, collecting decoction filtered, filtrate concentrates and add hydrochloric acid solution in the time of 70-80 ℃ regulates pH value to 1.0~3.0, insulation 1h left standstill 12 hours, filtered, precipitation adds 8~10 times of water gagings, regulate pH value to 6.0~8.0 with sodium hydroxide solution, add ethanol again and make and contain the alcohol amount and reach 40~60%, stir and make dissolving, added 50 ℃ of insulated and stirred of 0.1~1% active carbon 30 minutes, filter, filtrate is regulated pH value to 1.0~2.0,50 ℃ insulation 1 hour with hydrochloric acid solution, left standstill 10 hours, filter, it is 6.0~8.0 that precipitation is washed till pH value with ethanol, reclaims ethanol and obtains Radix Scutellariae extractum, drying under reduced pressure or spray drying get Radix Scutellariae extract.
Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) add water temperature and soak 30 minutes after, decoct secondary, each 2 hours, collecting decoction filtered, it is 1.20~1.25 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly add ethanol after the cooling and make and contain alcohol amount and reach 60~80%, fully stir, left standstill 12 hours, the leaching supernatant, regulate pH value to 6.0~8.0 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stirs evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extractum, drying under reduced pressure or spray drying obtain Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract.
After Fructus Forsythiae adds water temperature and soaks 30 minutes, decoct secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, it is 1.20~1.25 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly adds ethanol after the cooling and makes and contain the alcohol amount and reach 60~80%, fully stir, left standstill 12 hours, the leaching supernatant is regulated pH value to 6.0~8.0 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stir evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Fructus Forsythiae extractum, drying under reduced pressure or spray drying obtain Fructus Forsythiae extract.
Mix with toothpaste matrix according to the ratio that contains Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract 0.03~10g, Radix Scutellariae extract 0.03~10g, Fructus Forsythiae extract 0.03~10g among every 100g and to obtain the SHUANGHUANLIAN Chinese medicinal toothpaste.
Toothpaste matrix of the present invention is selected from abrasivus, wetting agent, thickening agent, adhesive, foaming agent, sweeting agent, antiseptic, aromatic, pH regulator agent, antioxidant, pigment, water and other additives.The amount of every kind of additive in Chinese medicinal toothpaste can change in the normal ranges of this area.
Suitable abrasivus can be selected silicon dioxide, calcium carbonate, calcium hydrogen phosphate and their combination for use, and consumption can be 0.5%~30% of toothpaste weight.
Suitable wetting agent can be selected sorbitol, silicon dioxide, PEG400, polyethylene glycol 1500, glycerol and their combination for use, and consumption can be 5%~80% of toothpaste weight.
Suitable thickening can be selected silicon dioxide, sodium carboxymethyl cellulose and their combination for use, and consumption can be 0.5%~15% of toothpaste weight.
Suitable adhesive can be selected xanthan gum, sodium carboxymethyl cellulose and their combination for use, and consumption can be 0.2%~2% of toothpaste weight.
Suitable foaming agent can be selected sodium lauryl sulphate for use, and consumption can be 1%~3% of toothpaste weight.
Suitable antiseptic can be selected benzoic acid, sodium benzoate, sorbic acid, potassium sorbate and their combination for use, and consumption can be 0.02%~0.3% of toothpaste weight.
Suitable sweeting agent can be selected saccharin sodium, xylitol, aspartame, steviol glycosides, sucralose and their combination for use, and consumption can be 0.03%~0.5% of toothpaste weight
Suitable pigment can be selected titanium dioxide, sodium copper chlorophllin, bright orchid and their combination for use, and consumption can be 0.02%~0.4% of toothpaste weight.
Suitable aromatic can be selected Ilicis Purpureae Herba Menthae essence, blue and white Herba Menthae essence for use, stay blue Herba Menthae essence, WS-3 essence and their combination, and when it existed, consumption can be 0.02%~2% of a toothpaste weight.
Suitable antioxidant can be selected BHT for use, and when it existed, consumption can be 0.01%~0.05% of a toothpaste weight.
Suitable pH regulator agent can be selected tetrasodium pyrophosphate, sodium hydroxide, sodium citrate, citric acid and their combination for use, and consumption can be 0.05%~2% of toothpaste weight.
The preparation process of toothpaste of the present invention comprises: can use any method that Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract, Radix Scutellariae extract, Fructus Forsythiae extract and suitable toothpaste additive are mixed, outgas through vacuum stirring, fill is sealed, promptly.One of preferred scheme is: Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract, Radix Scutellariae extract, Fructus Forsythiae extract and water, pH regulator agent, sweeting agent, antiseptic are mixed make water, wetting agent, adhesive, thickening agent, antioxidant, aromatic, pigment mix, make the polyhydric alcohol phase, water is mixed mutually with polyhydric alcohol, add abrasivus, foaming agent, aromatic mix homogeneously, through the vacuum stirring degassing, fill, seal, promptly.Another kind of preferred version is: Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract, Radix Scutellariae extract, Fructus Forsythiae extract, wetting agent, sweeting agent, pH regulator agent, foaming agent, aromatic mix, stir, mix with the solution of thickening agent, adhesive, adding abrasivus mixes, outgas through vacuum stirring, fill is sealed, promptly.
SHUANGHUANLIAN Chinese medicinal toothpaste among the present invention contains Radix Scutellariae, Flos Lonicerae (Flos Lonicerae, Flos Lonicerae), Fructus Forsythiae three flavor medicinal substances extracts, has biological effect widely, very strong antiinflammatory, antibiotic, antiviral, adjusting immunity is arranged and remove free radical antioxidative effect.Radix Scutellariae can also suppress cariogenic bacteria, and effectively the bacterium for degrading endotoxin can be used for the prevention and the treatment of periodontitis; Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) all has the different antibacterial action of degree to most of pathogen, and using Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) is the effective means of prevention and treatment oral disease as local application.Radix Scutellariae, Flos Lonicerae (Flos Lonicerae, Flos Lonicerae), Fructus Forsythiae all have heat-clearing and toxic substances removing, dispelling wind and heat pathogens effect.Three kinds of Chinese medicine extract are united the effect with Synergistic of using, and can effectively suppress in the oral cavity to produce the bacterial reproduction of abnormal flavour, in order to reduce the influence of Chinese medicine extract to mastic, improve the color and the character of toothpaste, make consumer more acceptant, in the extract preparation process: the Radix Scutellariae alcohol deposit fluid adds a certain amount of active carbon, be incubated decarburization at a certain temperature, Flos Lonicerae, Fructus Forsythiae extract respectively, in the precipitate with ethanol process, regulate pH, both keep the active component in the extract, reached satisfied refining effect again.The said extracted thing joined be prepared into the SHUANGHUANLIAN Chinese medicinal toothpaste in the suitable toothpaste matrix, has relevant pathogenic bacterium effect in the bacterial plaque of obvious suppression gingiva position through oral cavity antibacterial sensitization test proof, therefore can improve the gingiva relevant issues, eliminate or alleviate the halitosis that causes by oral cavity bacterium.
(4) specific embodiment
For example the present invention is done in more detail below and describes:
Example 1:
(1) prescription: the raw material of every 100g product consists of: Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) 5g, Radix Scutellariae 5g, Fructus Forsythiae 10g, sorbitol 20g, deionized water are an amount of, silica 1 0g, Polyethylene Glycol 1g, sodium lauryl sulphate 1g, sodium carboxymethyl cellulose 0.4g, xanthan gum 0.2g, saccharin sodium 0.03g, sodium benzoate 0.05g, titanium dioxide 0.1g, tetrasodium pyrophosphate 0.05g, blue and white Herba Menthae essence 0.05g, WS-3 essence 0.01g.
(2) preparation technology:
Radix Scutellariae decocts with water three times, and first, secondary each 2 hours, 1 hour for the third time, collecting decoction filters, and filtrate concentrates and add hydrochloric acid solution in the time of 70-80 ℃ regulates pH value to 1.0~2.0, insulation 1h left standstill 12 hours, filtered, precipitation adds 8 times of water gagings, regulate pH value to 6.0~7.0 with sodium hydroxide solution, add ethanol again and make and contain the alcohol amount and reach 40%, stir and make dissolving, added 50 ℃ of insulated and stirred of 0.2% active carbon 30 minutes, filter, filtrate is regulated pH value to 2.0 with hydrochloric acid solution, and 50 ℃ are incubated 1 hour, left standstill 10 hours, filter, it is 6.0~7.0 that precipitation is washed till pH value with ethanol, reclaims ethanol and obtains Radix Scutellariae extractum, drying under reduced pressure or spray drying get Radix Scutellariae extract; Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) add water temperature and soak 30 minutes after, decoct secondary, each 2 hours, collecting decoction filtered, it is 1.20 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly add ethanol after the cooling and make and contain alcohol amount and reach 60%, fully stir, left standstill 12 hours, the leaching supernatant, regulate pH value to 6.0~7.0 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stirs evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extractum, drying under reduced pressure obtains Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract; After Fructus Forsythiae adds water temperature and soaks 30 minutes, decoct secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, it is 1.20 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly adds ethanol after the cooling and makes and contain the alcohol amount and reach 60%, fully stir, left standstill 12 hours, the leaching supernatant is regulated pH value to 6.0~7.0 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stir evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Fructus Forsythiae extractum, drying under reduced pressure obtains Fructus Forsythiae extract; Flos Lonicerae extract, Radix Scutellariae extract, Fructus Forsythiae extract, tetrasodium pyrophosphate, saccharin sodium, sodium benzoate, an amount of mix homogeneously of deionized water are made water, WS-3 essence, Polyethylene Glycol, sodium carboxymethyl cellulose, xanthan gum, sorbitol, titanium dioxide, mix, make the polyhydric alcohol phase, water is joined polyhydric alcohol to mix in mutually, add silicon dioxide, sodium dodecyl sulfate solution, the abundant mix homogeneously of blue and white Herba Menthae essence, outgas through vacuum stirring, fill, seal, promptly.
Example 2:
(1) prescription: the raw material of every 100g product consists of: Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) 10g, Radix Scutellariae 5g, Fructus Forsythiae 5g, sorbitol 50g, deionized water are an amount of, silica 1 5g, Polyethylene Glycol 5g, sodium lauryl sulphate 2g, sodium carboxymethyl cellulose 0.6g, xanthan gum 0.4g, saccharin sodium 0.25g, potassium sorbate 0.02g, titanium dioxide 0.2g, tetrasodium pyrophosphate 0.1g, Ilicis Purpureae Herba Menthae essence 0.5g, BHT0.01g
(2) preparation technology
Radix Scutellariae decocts with water three times, and first, secondary each 2 hours, 1 hour for the third time, collecting decoction filters, and filtrate concentrates and add hydrochloric acid solution in the time of 70-80 ℃ regulates pH value to 1.5~2.0, insulation 1h left standstill 12 hours, filtered, precipitation adds 9 times of water gagings, regulate pH value to 6.5~7.5 with sodium hydroxide solution, add ethanol again and make and contain the alcohol amount and reach 50%, stir and make dissolving, added 50 ℃ of insulated and stirred of 0.5% active carbon 30 minutes, filter, filtrate is regulated pH value to 2.0 with hydrochloric acid solution, and 50 ℃ are incubated 1 hour, left standstill 10 hours, filter, it is 6.5~7.5 that precipitation is washed till pH value with ethanol, reclaims ethanol and obtains Radix Scutellariae extractum, drying under reduced pressure or spray drying get Radix Scutellariae extract; Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) add water temperature and soak 30 minutes after, decoct secondary, each 2 hours, collecting decoction filtered, it is 1.25 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly add ethanol after the cooling and make and contain alcohol amount and reach 75%, fully stir, left standstill 12 hours, the leaching supernatant, regulate pH value to 6.5~7.5 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stirs evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extractum, spray drying obtains Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract; After Fructus Forsythiae adds water temperature and soaks 30 minutes, decoct secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, it is 1.25 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly adds ethanol after the cooling and makes and contain the alcohol amount and reach 75%, fully stir, left standstill 12 hours, the leaching supernatant is regulated pH value to 6.5~7.5 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stir evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Fructus Forsythiae extractum, spray drying obtains Fructus Forsythiae extract; Flos Lonicerae extract, Radix Scutellariae extract, Fructus Forsythiae extract, tetrasodium pyrophosphate, saccharin sodium, potassium sorbate, an amount of mix homogeneously of deionized water are made water, BHT, Polyethylene Glycol, sodium carboxymethyl cellulose, xanthan gum, sorbitol, titanium dioxide, mix, make the polyhydric alcohol phase, water is joined polyhydric alcohol to mix in mutually, add silicon dioxide, sodium dodecyl sulfate solution, the abundant mix homogeneously of Ilicis Purpureae Herba Menthae essence, outgas through vacuum stirring, fill, seal, promptly.
Example 3:
(1) prescription: the raw material of every 100g product consists of: Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) 10g, Radix Scutellariae 10g, Fructus Forsythiae 10g, sorbitol 50g, deionized water are an amount of, silica 1 5g, sodium lauryl sulphate 2g, sodium carboxymethyl cellulose 0.6g, xanthan gum 0.4g, saccharin sodium 0.25g, sodium benzoate 0.1g, titanium dioxide 0.2g, sodium copper chlorophllin 0.05g, WS-3 essence 0.1g
(2) preparation technology
Radix Scutellariae decocts with water three times, first, secondary each 2 hours, 1 hour for the third time, collecting decoction filtered, filtrate concentrates and add hydrochloric acid solution in the time of 70-80 ℃ regulates pH value to 2.0~2.5, insulation 1h left standstill 12 hours, filtered, precipitation adds 10 times of water gagings, regulate pH value to 7.0~8.0 with sodium hydroxide solution, add ethanol again and make and contain the alcohol amount and reach 60%, stir and make dissolving, added 50 ℃ of insulated and stirred of 1% active carbon 30 minutes, filter, filtrate is regulated pH value to 1.5~2.0,50 ℃ insulation 1 hour with hydrochloric acid solution, left standstill 10 hours, filter, it is 7.0~8.0 that precipitation is washed till pH value with ethanol, reclaims ethanol and obtains Radix Scutellariae extractum, drying under reduced pressure or spray drying get Radix Scutellariae extract; Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) add water temperature and soak 30 minutes after, decoct secondary, each 2 hours, collecting decoction filtered, it is 1.20 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly add ethanol after the cooling and make and contain alcohol amount and reach 80%, fully stir, left standstill 12 hours, the leaching supernatant, regulate pH value to 7.0~8.0 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stirs evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extractum, drying under reduced pressure obtains Flos Lonicerae (Flos Lonicerae, Flos Lonicerae) extract; After Fructus Forsythiae adds water temperature and soaks 30 minutes, decoct secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction filters, and it is 1.25 clear paste that filtrate is concentrated into 70~80 ℃ relative density, slowly adding ethanol after the cooling makes and contains alcohol amount and reach 80%,, fully stir, left standstill 12 hours, the leaching supernatant, regulate pH value to 7.0~8.0 with sodium hydroxide solution, it is an amount of that residue adds 75% ethanol, stirs evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and obtain Fructus Forsythiae extractum, drying under reduced pressure or spray drying obtain Fructus Forsythiae extract; With Flos Lonicerae extract, Radix Scutellariae extract, Fructus Forsythiae extract, sorbitol, sodium lauryl sulphate, saccharin sodium, sodium benzoate, WS-3 essence, titanium dioxide, sodium copper chlorophllin, an amount of mix homogeneously of deionized water, mix with the aqueous solution of sodium carboxymethyl cellulose, xanthan gum, add the abundant mix homogeneously of silicon dioxide.Through the vacuum stirring degassing, fill is sealed, promptly.
Adopt the SHUANGHUANLIAN Chinese medicinal toothpaste that people's gingiva tissue inflammation and the relevant bacterium of product sulfide are carried out the oral cavity bacterium sensitization test: the unguentum of toothpaste sample dilutes 11 concentration with the continuous multiple of sterilized water.With porphyromonas gingivalis (P.gingivalis, P.g), the fertile Salmonella (P.intermedia of middle Prey, P.i), actinomyces viscosus (A.viscosus, A.v3 strain) culture is coated with bacterium in media surface, carry out the cylinder plate method test, through 37 ℃, anaerobism was cultivated 5 days, measure the antibacterial ring size of each concentration, determine the minimum inhibitory concentration (MIC) of each bacterium.The results are shown in Table 1:
Table 1
Experimental results show that: contain that SHUANGHUANLIAN effective ingredient toothpaste sample suppresses gingiva position bacterial plaque and relevant pathogenic bacterium effect obviously is better than the contrast toothpaste sample.