Background technology
Conventional oral care implement is mainly toothpaste, collutory etc. now, and its basic function is clean corona, and protection gingiva reduces oral cavity bacterium concentration with the generation of prevention oral disease.Along with growth in the living standard, the enhancing of health care consciousness.People propose more requirement to oral care implement, so on market, the oral care implement of main flow all adds the functional component of the various oral diseases of control, but are wherein the compound chemically synthesizing mostly.
Development along with the awareness of environment protection and health.Consumer more and more pays close attention to the safety of toothpaste, advocates natural and safe these two characteristics.Interpolation can effectively prevent and treat the toothpaste of the Chinese herbal medicine active component of oral disease, and because of its environmental protection, the features such as natural safety are subject to the favor of consumer, market to its demand also in continuous growth.
Oral cavity bacterium is the major reason that causes oral disease, and the Etiological of the oral diseases such as gingivitis, periodontitis, dental caries, dental calculus, dental plaque, gingival hemorrhage, dentine hypersensitivity and halitosis is that antibacterial is at the intraoral quantity amount reproduction that causes out of control.Reduce oral cavity bacterium concentration and can fundamentally safeguard oral health.
Along with the development of modern Separation of Natural Products and detection technique, Ganoderma is with a long history as one, Chinese medicine safely and effectively, and the effect of its active component is through multi-party verification.And one of active component in Ganoderma ganoderan, existing bibliographical information finds to have significant bacteriostasis, and (" ganoderan Bacteriostatic Activities [J] " < < North China agronomy is reported > > 2008, (23): 282-285, " research of ganoderan bacteriostasis [J] " < < edible fungi > > 2012 (2): 60-64) this lays the first stone for the application of Ganoderma in oral care implement, make it have the prospect of preparation Ganoderma toothpaste.
Chewing gum (publication number CN00123055 and CN200710010025) containing Ganoderma composition in retrieval Chinese patent belongs to leisure food, to oral cavity cleaning, can only play assosting effect.And consumer orientation is in using the toothpaste of daily indispensability to keep oral cavity cleaning health, adopt the toothpaste of inclusion enclave parcel Ganoderma and other compositions (publication number CN201310413888) thereof, its complex process, high expensive; Separately because the cleaning oral cavity step time such as brush teeth in daily life is shorter, and the effect of the microcapsule technology such as inclusion enclave is embedding and delays to discharge (" in the progress of microcapsule structure and performance [J] " < < Chinese biological engineering magazine > > 2010,30 (1): 104-110), therefore in shorter brushing time, the Ganoderma active ingredient in microcapsule is difficult to play a role.
Summary of the invention
The object of the invention is blank and the weak point in toothpaste application in the past for Ganoderma, a kind of effective component of glossy ganoderma that contains is provided, and can participates in fast cleaning teeth, the Ganoderma toothpaste of performance bacteriostasis.
The technical solution adopted in the present invention is a kind of Ganoderma toothpaste, the substrate abrasivus that it contains toothpaste necessity, foaming agent, wetting agent, pure water etc., and its main points are to contain in every 100g toothpaste the pure extract 0.5-5g of Ganoderma.
The present invention adds the pure extract of Ganoderma in the composition of existing toothpaste, utilizes the significant bacteriostasis of ganoderan to reduce oral cavity bacterium concentration, fundamentally safeguards oral health.
The pure extraction product of wherein said Ganoderma is adopted with the following method and is obtained: the water extraction liquid of Ganoderma sporophore or Ganoderma spore powder is separated with ultrafilter membrane through ceramic membrane, and ceramic membrane interception molecular weight is 1 * 10
5, ultrafilter membrane molecular cut off is 5000, the molecular weight obtaining between the two is 5000-1 * 10
5trapped fluid; 1 volume trapped fluid is joined to the AB-8 macroporous resin column internal adsorption of 1 volume, use 3 volume 50% alcoholic solution eluting, collect the concentrated oven dry of eluent, be the pure extract of Ganoderma, in this extract, the content of ganoderan reaches 37-42%.
The present invention, by repeatedly testing, obtains the molecular weight of extract between 5000-1 * 10
5between time, contained ganoderan effective ingredient is the most concentrated, with it, is added in toothpaste, the characteristic that makes full use of the significant bacteriostasis of ganoderan reduces oral cavity bacterium concentration, fundamentally safeguards oral health.
The water extraction liquid of described Ganoderma sporophore or Ganoderma spore powder refers to by 1 part of Ganoderma sporophore or Ganoderma spore powder and adds 10-20 part pure water, 80-100 ℃ of lixiviate 2-4 hour, and filtration or centrifugal, obtains filtrate; Again every part of filtering residue is added to 10-20 part pure water, 80-100 ℃ of lixiviate 2-4 hour, filtration or centrifugal, merges 2 filtrates and is water extraction liquid.
Membrane separation technique is a kind of isolation technics of emerging emergence: have separation, concentrated, purification and refining function concurrently, efficiently, realizing molecular level when energy-saving and environmental protection filters, membrane separation technique can effectively be removed the impurity in Ganoderma extract, improve active constituent content in Ganoderma extract, in enclosed environment, operation is to avoid bringing into Pollution by Chemicals, separated to avoid destroying effective ingredient at normal temperatures.
Ganoderma sporophore of the present invention or Ganoderma spore powder refer to sporophore or the Ganoderma spore powder of basidiomycetes Aphyllophorales Ganodermataceae Ganoderma fungus Ganoderma (another name Ganoderma lucidum (Leyss. Ex Fr.) Karst.) (Ganoderma lucidun) or Ganoderma (Ganaderma sinense) (calling wooden sesame).
The pure extract of Ganoderma of the present invention refers to the active component being obtained by the sporophore of basidiomycetes Aphyllophorales Ganodermataceae Ganoderma fungus Ganoderma (another name Ganoderma lucidum (Leyss. Ex Fr.) Karst.) (Ganoderma lucidun) or Ganoderma (Ganaderma sinense) (calling wooden sesame) or Ganoderma spore powder extraction and purification, and form is including but not limited to solution, extractum and fine powder; The extracting method of the pure extract of Ganoderma comprises but is not limited to said method, can also adopt the additive method of supercritical extraction, microwave extraction to extract then and obtain through membrance separation and macroporous resin eluting;
Toothpaste of the present invention can also contain other Chinese herbal medicine extracts, such as Flos Lonicerae, Cortex Magnoliae Officinalis or Cortex Moutan etc.;
The preparation technology of Ganoderma toothpaste is:
Under room temperature, directly the liquid materials such as the pure water measuring, wetting agent, sweeting agent, the pure extract of Ganoderma and other Chinese medicine extract are added temporary cylinder to mix; Add pre-dispersed still carry out pre-dispersed and mix the powders such as the abrasivus measuring, adhesive, foaming agent; Open cream still vacuum pump and suck above-mentioned liquid material; Open scraper, enter above-mentioned powder, drive agitator and colloid mill, after 60 minutes, drop into essence, after 10 minutes, close successively colloid mill, agitator, scraper, vacuum breaker, stop vacuum pump, drive still and obtain lotion of toothpaste.
The present invention is the pure extract of the high Ganoderma of content that adds ganoderan in the composition of existing toothpaste, utilizes the significant bacteriostasis of ganoderan to reduce oral cavity bacterium concentration, fundamentally safeguards oral health.
The specific embodiment
Below in conjunction with embodiment, the present invention is further illustrated, and in following each embodiment, related percentage ratio except as otherwise noted, otherwise is all that percentage ratio with weight calculates.
Consumption for each active ingredient in can more clear embodiment 1-3, is listed as follows:
The toothpaste constitutive material of embodiment 1-3 and weight percent content are as following table:
Embodiment 1, and a kind of Ganoderma toothpaste contains the pure extract 0.5g of Ganoderma in every 100g Ganoderma toothpaste.The pure extract of described Ganoderma is to adopt the pure extract obtaining with the following method: 1 part of Ganoderma sporophore or Ganoderma spore powder add 20 parts of pure water, and 80 ℃ of lixiviates 4 hours are filtered or centrifugal, obtain filtrate; The filtering residue of gained is added to 20 parts of pure water, 80 ℃ of lixiviates 4 hours, filter or centrifugal, merge 2 times filtrate again, and separated with ultrafilter membrane through ceramic membrane, ceramic membrane interception molecular weight is 1 * 10
5, ultrafilter membrane molecular cut off is 5000, the molecular weight obtaining between the two is 5000-1 * 10
5trapped fluid, 1 volume trapped fluid is added to the AB-8 macroporous resin column internal adsorption of 1 volume, use 3 volume 50% alcoholic solution eluting, collect that eluent is concentrated dries, be the pure extract of Ganoderma.
Under room temperature, directly add temporary cylinder to mix the liquid materials such as 1 part of 28.5 parts of the pure water measuring, 15 parts of wetting agent glycerol, 25 parts of sweeting agent sorbitol and 5 parts of xylitol, 5 parts of the pure extracts of Ganoderma and Flos Lonicerae extract; Add pre-dispersed still carry out pre-dispersed and mix the powders such as 5 parts of the abrasivus silica 1s measuring, 1.2 parts of adhesive xanthan gum, 2 parts of foaming agent sodium lauryl sulphates; Open cream still vacuum pump and suck above-mentioned liquid material; Open scraper, enter above-mentioned powder, drive agitator and colloid mill, after 60 minutes, drop into 0.7 part of 0.1 part of essence Mentholum and Oleum menthae, after 10 minutes, close successively colloid mill, agitator, scraper, vacuum breaker, stop vacuum pump, drive still and obtain lotion of toothpaste;
Wetting agent is except being used glycerol, also available sorbitol, propylene glycol or Polyethylene Glycol etc.;
Sweeting agent is except being used sorbitol, also available xylitol, mannitol or saccharin sodium etc.;
Abrasivus is except being used silicon dioxide, also available calcium carbonate, calcium pyrophosphate or silicate hydrate etc.;
Adhesive is except being used xanthan gum, also available sodium carboxymethyl cellulose, carrageenan or guar gum etc.;
Foaming agent is except being used sodium lauryl sulphate, also available sodium laurylsulfate or 2-acyl-oxygen base key sodium sulfonate etc.
Embodiment 2, and a kind of Ganoderma toothpaste contains the pure extract 2.5g of Ganoderma in every 100g Ganoderma toothpaste.The pure extract of described Ganoderma is to adopt the pure extract obtaining with the following method: 1kg Ganoderma sporophore or Ganoderma spore powder add 10 kg pure water, and 100 ℃ of lixiviates 2 hours are filtered or centrifugal, obtain filtrate; Again resulting filtering residue is added to 10 kg pure water, 100 ℃ of lixiviates 2 hours, filter or centrifugal, merge 2 times filtrate, separated with ultrafilter membrane through ceramic membrane, ceramic membrane interception molecular weight is 1 * 105, and ultrafilter membrane molecular cut off is 5000, obtains the trapped fluid that the molecular weight between the two is 5000-1 * 105,1 volume trapped fluid adds the AB-8 macroporous resin column internal adsorption of 1 volume, use 3 volume 50% alcoholic solution eluting, collect the concentrated oven dry of eluent, be the pure extract of Ganoderma.
Similar with existing toothpaste processing technology: under room temperature, directly to add temporary cylinder to mix the liquid materials such as 2 parts of 32.5 parts of the pure water measuring, 15 parts of wetting agent glycerol, 30 parts of sweeting agent sorbitol and 5 parts of xylitol, 1 part of magnolia obovata extracts of the pure extract of Ganoderma; Add pre-dispersed still carry out pre-dispersed and mix the powders such as 5 parts of the abrasivus silica 1s measuring, 1.2 parts of adhesive xanthan gum, 2 parts of foaming agent sodium lauryl sulphates; Open cream still vacuum pump and suck above-mentioned liquid material; Open scraper, enter above-mentioned powder, drive agitator and colloid mill, after 60 minutes, drop into 0.7 part of 0.1 part of essence Mentholum and Oleum menthae, after 10 minutes, close successively colloid mill, agitator, scraper, vacuum breaker, stop vacuum pump, drive still and obtain lotion of toothpaste; It is identical with upper example that all the other do not state part.
Embodiment 3, and a kind of Ganoderma toothpaste contains the pure extract 5g of Ganoderma in every 100g Ganoderma toothpaste.The pure extract of described Ganoderma is to adopt the pure extract obtaining with the following method: 1 part of Ganoderma sporophore or Ganoderma spore powder add 15 parts of pure water, and 90 ℃ of lixiviates 3 hours are filtered or centrifugal, obtain filtrate; Again 1 part of filtering residue is added to 15 parts of pure water, 90 ℃ of lixiviates 3 hours, filter or centrifugal, merge 2 times filtrate, and separated with ultrafilter membrane through ceramic membrane, ceramic membrane interception molecular weight is 1 * 10
5, ultrafilter membrane molecular cut off is 5000, the molecular weight obtaining between the two is 5000-1 * 10
5trapped fluid, 1 volume trapped fluid adds the AB-8 macroporous resin column internal adsorption of 1 volume, uses 3 volume 50% alcoholic solution eluting, collects that eluent is concentrated dries, and is the pure extract of Ganoderma.Under room temperature, directly add temporary cylinder to mix the liquid materials such as 0.5 part of 35.5 parts of the pure water measuring, 15 parts of wetting agent glycerol, 20 parts of sweeting agent sorbitol and 5 parts of xylitol, 10 parts of the pure extracts of Ganoderma and Cortex Moutan extract; Add pre-dispersed still carry out pre-dispersed and mix the powders such as 5 parts of the abrasivus silica 1s measuring, 1.2 parts of adhesive xanthan gum, 2 parts of foaming agent sodium lauryl sulphates; Open cream still vacuum pump and suck above-mentioned liquid material; Open scraper, enter above-mentioned powder, drive agitator and colloid mill, after 60 minutes, drop into 0.7 part of 0.1 part of essence Mentholum and Oleum menthae, after 10 minutes, close successively colloid mill, agitator, scraper, vacuum breaker, stop vacuum pump, drive still and obtain lotion of toothpaste.It is identical with embodiment 1 that all the other do not state part.
Sampling detects, use 2010 editions Firsts of < < " Ganoderma [M] " < < Chinese Pharmacopoeia > >, sulphuric acid-anthrone method of recording in 174-175 > > detects the purity of the ganoderan of the extract of each step of the present invention, draw: at water extraction liquid, drying the ganoderan purity obtaining in extractum is 11-13%, through the ceramic membrane trapped fluid separated with ultrafilter membrane, drying ganoderan purity in the extractum obtaining is 21-25%, through the eluent of AB-8 macroporous resin column internal adsorption, concentrated to dry ganoderan purity in the pure extract of Ganoderma obtaining be 37-42%.
The assay of high performance liquid chromatograph-evaporative light scattering detector coupling (HPLC-ELSD) shows: in the pure extract of Ganoderma, retained most ganoderan (Fig. 1, Fig. 2), the above results shows that the purity of ganoderan in the pure extract of Ganoderma of the present invention is the highest, and fungistatic effect is better.
The assay method of the finger printing of the HPLC-ELSD of this pure extract is:
1. instrument and reagent
Shimadzu LC-20A, purified water.
2. chromatographic condition
Mobile phase: purified water;
Pillar: gel chromatographic columns TSK Gel G4000 PWXL(7.8*300)
Flow velocity: 1mL/min;
Drift tube temperature: 60 degree;
Air-flow velocity: 2ml/min;
Gain: 1;
Sampling volume: 20 μ L.
3. finger print identification: see Fig. 1, Fig. 2.Fig. 1 is Ganoderma water extract HPLC-ELSD finger printing (vertical coordinate is ganoderan response value 140mv, extension rate * 1); Fig. 2 is the pure extractive HPLC-ELSD of Ganoderma finger printing (vertical coordinate is ganoderan response value 160mv, extension rate * 5).
4. by Fig. 1 and Fig. 2 contrast, can be found out: the peak type of the pure extract of Ganoderma approaches Ganoderma water extract, but membrance separation is removed impurity and a small amount of polysaccharide of 7.1min macromolecule before, retained most of ganoderan of 7.1min-10.9min; Dilute the peak height (response value 140mv) that the pure extract peak height of Ganoderma (response value 160mv) of 5 times is still greater than Ganoderma water extract simultaneously, illustrate that the polyoses content of the pure extract of Ganoderma obtaining is significantly higher than Ganoderma water extract after membrance separation and purification by macroporous resin two steps.
Above according to illustrative embodiment, present invention is described, but should understand the restriction that the present invention is not subject to embodiment.Conversion and modification that those skilled in the art may make by reading description also fall in the scope of the invention of appended claims definition.