CN103191036A - Sweet tea extract-contained toothpaste - Google Patents
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Abstract
The invention provides sweet tea extract-contained toothpaste. The toothpaste comprises a sweetening agent, wherein the sweetening agent is a sweet tea extract which is 0.01-0.1% of the toothpaste based on weight, the sweet tea extract contains 5-40% of rubusoside, and 2-21% of weet tea polyphenol. The sweet ingredient in the sweet tea extract-contained toothpaste is the sweet tea extract, when the rubusoside content in the sweet tea extract is within the range of 5-40% and the sweet tea polyphenol in the sweet tea extract is within the range of 2-21%, the rubusoside and the sweet tea polyphenol interact to achieve the effect of well preventing tooth decay and improving oral cavity health, and when the sweet tea extract content in the toothpaste is certain, the effect of preventing the tooth decay of the toothpaste is improved along with the reduction of the rubusoside content and the increase of the sweet tea polyphenol content.
Description
Technical field
The daily-use chemical industry technical field that belongs to of the present invention is specifically related to a kind of toothpaste that contains sweet tea extract.
Background technology
Toothpaste is made of abrasivus, wetting agent, surfactant, binding agent, spice, sweeting agent and water.Sweeting agent can improve the mouthfeel of toothpaste, generally selects glucide or xylitol, and the sugariness height of glucide is 300~500 times of sucrose, but take in for a long time or take in a large number health is harmful to.Xylitol has advantages such as sugariness height, heat are low, but excessive absorption xylitol, can cause that triglyceride raises in the blood of human body, causes coronary atherosclerosis, also might cause diseases such as abdominal discomfort, flatulence, diarrhoea.
Folium hydrangeae strigosae (Rubus Suavissmus S Lee) is the distinctive natural sweet taste plant in Guangxi, also is best in the world Gao Tian, low grade fever, safety non-toxic and the sweet taste plant with health care.Contain approximately in the Folium hydrangeae strigosae more than 3.2% flavone compound, about 9% sweet tea tannins and 5~8% glycosides (Rubusoside), in addition, also be rich in several amino acids and necessary for human body trace element, have higher nutritive value and health care value.Glycosides is the sweet taste factor that Folium hydrangeae strigosae presents the sweet taste mouthfeel, and it is the low in calories high sweet substance of the diterpene glycoside of steviol (Steviol) and glucose be combined into, and its molecular formula is C
32H
50O
12The glycosides that extracts from Folium hydrangeae strigosae is mouthfeel the best in the sweet taste plant, and the pure degree of sweet taste is near white sugar, and its sugariness is equivalent to 300 times of sucrose, is sugared Dai Pin best in the Nature.Glycosides can also suppress in the oral cavity to produce the activity of the glucosyltransferase (GTF) of Streptococcus mutans (S.mutans) growth of dental caries and synthetic glucosan, thereby suppress the water-insoluble glucan (WIG) of strong adhesion and the generation of acid, prevent the generation of dental plaque, reach the effect of caries prevention.Sweet tea tannins is active component important in the Folium hydrangeae strigosae, comprise distinctive GOD type elladitannin, also comprise gallic acid, ellagic acid, 2-pyrone-4, the 6-dicarboxylic acids, brevifolin carboxylic acid, sanguisorbic acid dilactone, caffeic acid etc., having low density lipoprotein, LDL in obvious antioxidation, mutation, cholesterol reducing, the reduction blood, suppress increased blood pressure, suppress that blood glucose rises, suppresses platelet aggregation, antibiotic, anti-food anaphylaxis, improves the intestines and stomach microbial environment, the smelly effect that disappears, is to find optimal natural antioxidant at present.Therefore, sweet tea extract is a kind of desirable sweeting agent, can be applied to the toothpaste production field.
The document " glycosides and xylitol are to the comparative study of the insoluble extracellular polysaccharide of Streptococcus mutans synthetic water " that is published in the 32nd the 3rd phase of volume of " Guangxi medical science " March in 2010 is to be raw material with the glycosides, with the tryptone-tryptose that contains 0.5% sucrose-yeast extract medium (TTY), adopt doubling dilution to be made into the glycosides solution of 5 kinds of variable concentrations, be followed successively by 5g/100ml, 2.5g/100ml, 0.125g/100ml, 0.625g/100ml, 0.313g/100ml, the glycosides solution of above-mentioned concentration has all produced certain inhibitory action to the insoluble extracellular polysaccharide of Streptococcus mutans synthetic water, in above-mentioned concentration range, along with the reduction of glycosides concentration, inhibition descends.The document " Folium hydrangeae strigosae tooth protection sheet is to the influence of glucosyltransferase and extracellular water-insoluble polysaccharide " that is published in the 34th the 6th phase of volume of " Guangxi medical science " June in 2012 is that the Folium hydrangeae strigosae tooth protection buccal tablet with the natural company limited production of Guilin collection fine jade strength is raw material, with the tryptone-tryptose that contains 1% sucrose-yeast extract medium (TTY), adopt doubling dilution to be made into the solution of 5 kinds of variable concentrations, be followed successively by 5g/50ml, 2.5g/50ml, 1.250g/50ml, 0.625g/50ml, 0.313g/50ml, because the content of glycosides is 5.5% in this Folium hydrangeae strigosae tooth protection buccal tablet, be converted into the concentration of glycosides, be followed successively by 0.275g/50ml, 0.138g/50ml, 0.068g/50ml, 0.034g/50ml, 0.017g/50ml, the Folium hydrangeae strigosae tooth protection buccal tablet of above-mentioned concentration has obvious inhibitory action to Streptococcus mutans GTF enzyme activity, also can suppress the synthetic of WIG, in above-mentioned concentration range, along with the reduction of glycosides concentration, inhibition descends.Comprehensive above-mentioned two pieces of documents, we can draw a conclusion, and namely glycosides concentration is more high, and is more strong to the inhibition of Streptococcus mutans, otherwise, then more weak.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of toothpaste that contains sweet tea extract, this toothpaste is sweet ingredient with the sweet tea extract, when containing than the glycosides of low dosage and higher dosage sweet tea tannins in the sweet tea extract, the effect that can reach caries prevention preferably and improve oral health.
Technical scheme provided by the invention is a kind of toothpaste that contains sweet tea extract, comprises sweeting agent, and described sweeting agent is sweet tea extract, and it accounts for 0.2~2.5% of this toothpaste weight; The weight content of glycosides is 5~40% in the described sweet tea extract, and the weight content of sweet tea tannins is 2~21%.
Sweet tea extract of the present invention accounts for 2~2.5% of this toothpaste weight.
Sweet tea extract of the present invention accounts for 2.5% of this toothpaste weight.
The weight content of glycosides is 5~40% in the sweet tea extract of the present invention, and the weight content of sweet tea tannins is 7~21%.
The weight content of glycosides is 5~40% in the sweet tea extract of the present invention, and the weight content of sweet tea tannins is 15~21%.
The weight content of glycosides is 5~35% in the sweet tea extract of the present invention, and the weight content of sweet tea tannins is 16~21%.
The weight content of glycosides is 5~30% in the sweet tea extract of the present invention, and the weight content of sweet tea tannins is 17~21%.
The weight content of glycosides is 5~20% in the sweet tea extract of the present invention, and the weight content of sweet tea tannins is 18~21%.
The weight content of glycosides is 5~10% in the sweet tea extract of the present invention, and the weight content of sweet tea tannins is 18~21%.
The weight content of glycosides is 5% in the sweet tea extract of the present invention, and the weight content of sweet tea tannins is 21%.
Toothpaste of the present invention also comprises abrasivus, wetting agent, surfactant, binding agent, spice and water.Abrasivus can be calcium carbonate, dicalcium phosphate dehydrate, calcium phosphate dibasic anhydrous, calcium pyrophosphate, silicate hydrate or aluminium hydroxide.Wetting agent can be glycerol, propylene glycol or sorbitol.Surfactant generally adopts neutral detergent--sodium lauryl sulfonate, can foam the dirt in rinsing the mouth again, free from extraneous odour.Binding agent can make to prepare burden in the toothpaste and be uniformly dispersed, and generally adopts sanlose and derivant thereof or sodium alginate.Spice is generally pennyroyal spice, specifically is Oleum menthae, Mentholum, and can give toothpaste and clearly feel, also can be fruits essence, as citrus flavor etc.
The applicant finds, when adopting glycosides content 5~40%, the sweet tea extract of sweet tea tannins content in 2~21% scope is during as the sweeting agent of toothpaste, make toothpaste have suitable sweet taste on the one hand, to adapt to part crowd's mouthfeel needs, on the other hand, in the sweet tea extract glycosides and sweet tea tannins with the contact process in oral cavity in, can play synergism, give full play to the effect of the activity of the glucosyltransferase (GTF) that suppresses the degeneration streptococcus growth and reduce synthetic glucosan, thereby reach the water-insoluble glucan (WIG) and sour the telling on that suppress strong adhesion, prevent that dental plaque from producing, and then reach the effect of caries prevention.The applicant also finds, in toothpaste the content one of sweet tea extract regularly, the caries prevention effect reduces along with the rising of glycosides content in the sweet tea extract, reducing of sweet tea tannins content.
The specific embodiment
The present invention is further elaborated for following specific embodiment, but not as a limitation of the invention.
Following percent is percetage by weight.
Embodiment 1
The formulation of toothpaste that contains sweet tea extract: 0.2 part of sweet tea extract, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 27.8 parts in water.
The weight content of glycosides is 40% in the described sweet tea extract, sweet tea tannins is 21%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 40 orders, put into 30%(v/v) ethanol, be 40 ℃ of following reflux, extract, 2 times in ultrasound wave 40KHz, temperature, extract 20min at every turn, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 9, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 70%(v/v) ethanol elution, get eluent and concentrate, drying is sweet tea extract, wherein, the weight content of glycosides is 40%, the weight content of sweet tea tannins is 21%.
Embodiment 2
The formulation of toothpaste that contains sweet tea extract: 2.5 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 25.5 parts in water.
The weight content of glycosides is 5% in the described sweet tea extract, the content of sweet tea tannins is 2%.
The preparation method of described sweet tea extract:
Get sweet tea and be crushed to 5 orders, put into 80 ℃ of water lixiviates 2 times, each lixiviate 20min, merge extractive liquid, filters, and concentrates, and drying is sweet tea extract, and wherein, the weight content of glycosides is 5%, the weight content of sweet tea tannins is 2%.
Embodiment 3
The formulation of toothpaste that contains sweet tea extract: 2 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26 parts in water.
The weight content of glycosides is 5% in the described sweet tea extract, sweet tea tannins is 21%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 20 orders, put into 10%(v/v) ethanol, room temperature lixiviate 2 times, each lixiviate 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) with the D101 macroporous adsorbent resin Folium hydrangeae strigosae crude extract is carried out adsorbing separation, uses 50%(v/v) ethanol elution, to get eluent and concentrate, drying is sweet tea extract, and wherein, the weight content of glycosides is 5%, the weight content of sweet tea tannins is 21%.
Embodiment 4
The formulation of toothpaste that contains sweet tea extract: 2 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26 parts in water.
The weight content of glycosides is 10% in the described sweet tea extract, sweet tea tannins is 18%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 30 orders, put into 30%(v/v) ethanol, room temperature lixiviate 2 times, each lixiviate 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) with the D101 macroporous adsorbent resin Folium hydrangeae strigosae crude extract is carried out adsorbing separation, uses 50%(v/v) ethanol elution, eluent is concentrated, drying is sweet tea extract, and wherein, the weight content of glycosides is 10%, the weight content of sweet tea tannins is 18%.
Embodiment 5
The formulation of toothpaste that contains sweet tea extract: 2 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26 parts in water.
The weight content of glycosides is 40% in the described sweet tea extract, sweet tea tannins is 15%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 40 orders, put into 30%(v/v) ethanol, be 40 ℃ of following lixiviates 2 times in ultrasound wave 40KHz, temperature, each lixiviate 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 11, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 70%(v/v) ethanol elution, eluent is concentrated, and drying is sweet tea extract, wherein, the weight content of glycosides is 40%, the weight content of sweet tea tannins is 15%.
Comparative examples 1
The formulation of toothpaste that contains sweet tea extract: 2 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26 parts in water.
The weight content of glycosides is 70% in the described sweet tea extract, sweet tea tannins is 7%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 40 orders, add water and mix, add the cellulase of sweet tea weight 0.3%, enzymolysis is 2 hours under 40 ℃ of temperature, pH4.5 condition, and enzyme denaturing filters, and gets filtrate;
2) be that the macromolecular filtering film of 10,000 molecular weight separates with filtrate by the aperture, obtain separating medium;
3) separating medium is carried out adsorbing separation with anion exchange resin, obtain separating medium for the second time, separating medium carries out adsorbing separation by ADS-7 type macroporous adsorbent resin for the second time again, use 50%(v/v then) ethanol elution, it is concentrated, dry to get eluent, be sweet tea extract, wherein, the weight content of glycosides is 70%, the weight content of sweet tea tannins is 7%.
Comparative examples 2
The formulation of toothpaste that contains sweet tea extract: 2 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26 parts in water.
The weight content of glycosides is 95% in the described sweet tea extract, sweet tea tannins is 2%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 40 orders, add water and mix, add the cellulase of sweet tea weight 0.5%, the compound enzyme of hemicellulase, enzymolysis is 3 hours under 40 ℃ of temperature, pH4.5 condition, and enzyme denaturing filters, and gets filtrate;
2) be that the hollow ceramic film device that can hold back 10,000 molecular weight carries out ultra-filtration and separation with filtrate by the aperture, get trapped fluid and separating medium;
3) separating medium is carried out adsorbing separation by anion exchange resin, obtain separating medium for the second time, separating medium carries out adsorbing separation by ADS-7 type macroporous adsorbent resin for the second time again, use 70%(v/v then) ethanol elution, eluent is concentrated, and drying is sweet tea extract, wherein, the weight content of glycosides is 95%, the weight content of sweet tea tannins is 2%.
Embodiment 6
The formulation of toothpaste that contains sweet tea extract: 1.5 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26.5 parts in water.
The weight content of glycosides is 35% in the described sweet tea extract, sweet tea tannins is 16%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 30 orders, put into 20%(v/v) ethanol, be 40 ℃ of following lixiviates 2 times in ultrasound wave 30KHz, temperature, each 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 10.5, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 60%(v/v) ethanol elution, get eluent and concentrate, drying is sweet tea extract, wherein, the weight content of glycosides is 35%, the weight content of sweet tea tannins is 16%.
Embodiment 7
The formulation of toothpaste that contains sweet tea extract: 0.5 part of sweet tea extract, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 27.5 parts in water.
The weight content of glycosides is 20% in the described sweet tea extract, sweet tea tannins is 20%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 20 orders, put into 30%(v/v) ethanol, be lixiviate 20min under 40 ℃ of conditions in temperature, filter, get filtrate and reclaim solvent, get the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 10, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 50%(v/v) ethanol elution, get eluent and concentrate, drying is sweet tea extract, wherein, the weight content of glycosides is 20%, the weight content of sweet tea tannins is 20%.
Embodiment 8
The formulation of toothpaste that contains sweet tea extract: 1.8 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26.2 parts in water.
The weight content of glycosides is 30% in the described sweet tea extract, sweet tea tannins is 19%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 30 orders, put into 10%(v/v) ethanol, be lixiviate 2 times under 30 ℃ of conditions in ultrasound wave 20KHz, temperature, each 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 10.8, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 50%(v/v) ethanol elution, get eluent and concentrate, drying is sweet tea extract, wherein, the weight content of glycosides is 30%, the weight content of sweet tea tannins is 19%.
Embodiment 9
The formulation of toothpaste that contains sweet tea extract: 1 part of sweet tea extract, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 27 parts in water.
The weight content of glycosides is 8.9% in the described sweet tea extract, sweet tea tannins is 20.2%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 30 orders, put into 20%(v/v) ethanol, room temperature lixiviate 2 times, each 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 9.5, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 60%(v/v) ethanol elution, get eluent and concentrate, drying is sweet tea extract, wherein, the weight content of glycosides is 8.9%, the weight content of sweet tea tannins is 20.2%.
Embodiment 10
The formulation of toothpaste that contains sweet tea extract: 0.3 part of sweet tea extract, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 27.7 parts in water.
The weight content of glycosides is 5% in the described sweet tea extract, sweet tea tannins is 5%.
The preparation method of described sweet tea extract:
Get sweet tea and be crushed to 5 orders, put into 80 ℃ of water lixiviate 30min, merge extractive liquid, filters, and concentrates, and drying is sweet tea extract, and wherein, the weight content of glycosides is 5%, the weight content of sweet tea tannins is 5%.
Embodiment 11
The formulation of toothpaste that contains sweet tea extract: 1.2 parts of sweet tea extracts, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 26.8 parts in water.
The weight content of glycosides is 40% in the described sweet tea extract, sweet tea tannins is 7%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 40 orders, put into 30%(v/v) ethanol, be 70 ℃ of following lixiviates 2 times in ultrasound wave 40KHz, temperature, each lixiviate 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 12.5, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 50%(v/v) ethanol elution, eluent is concentrated, and drying is sweet tea extract, wherein, the weight content of glycosides is 40%, the weight content of sweet tea tannins is 7%.
Embodiment 12
The formulation of toothpaste that contains sweet tea extract: 0.4 part of sweet tea extract, 45 parts of dicalcium phosphate dehydrate, 10 parts of glycerol, 10 parts of sorbitol, 1 part of carboxymethyl cellulose, 5 parts of sodium laurylsulfates, 1 part of Mentholum, 27.6 parts in water.
The weight content of glycosides is 40% in the described sweet tea extract, sweet tea tannins is 10%.
The preparation method of described sweet tea extract:
1) get sweet tea and be crushed to 40 orders, put into 30%(v/v) ethanol, be 60 ℃ of following lixiviates 2 times in ultrasound wave 40KHz, temperature, each lixiviate 20min, merge extractive liquid, filters, and gets filtrate and reclaims solvent, gets the Folium hydrangeae strigosae crude extract.
2) adding lime water in the Folium hydrangeae strigosae crude extract, to make its pH value be 11, treat contamination precipitation after, the elimination precipitation, it is standby to get supernatant.
3) regulate supernatant pH to neutrality, with the D101 macroporous adsorbent resin it carried out adsorbing separation, use 50%(v/v) ethanol elution, eluent is concentrated, and drying is sweet tea extract, wherein, the weight content of glycosides is 40%, the weight content of sweet tea tannins is 10%.
Embodiment 1~12 and comparative examples 1~2 described toothpaste all prepare according to a conventional method.
Experimental example
For showing the toothpaste of sweet tea extract that contains of the present invention to the preventive effect of dental caries, the applicant has carried out experiment in vitro research at this toothpaste to the mechanism of action of cariogenic bacteria (Streptococcus mutans), specifically is reported as follows:
1, experimental technique
1.1 the preparation of toothpaste solution and bacteria suspension
Experimental group: the toothpaste 125g that gets the embodiment of the invention 3~5 and comparative examples 1~2 respectively, with its pulverizing, place test tube, add the TTY fluid medium (tryptone-tryptose-yeast extract medium) that 100ml contains 1% sucrose more respectively and be made into toothpaste solution.
Negative control group: adopt the TTY fluid medium that does not contain this toothpaste.
With Streptococcus mutans (S.mutans) behind TSB culture medium (trypsinization Semen sojae atricolor fluid medium) activation 3h, being inoculated in 37 ℃ of following anaerobism of MSB solid medium (light saliva is selected culture medium) cultivated 48 hours, the picking colonies typical is made suspension in the 5ml physiological saline solution, harmonic length is the 540nm place, (Optical Density OD) is 1.0 bacteria suspension to optical density value.
1.2, toothpaste solution is to the influence of cariogenic bacteria growth
Get the 0.3ml bacterial suspension inoculation respectively in the toothpaste solution of 3ml variable concentrations, 37 ℃ of following anaerobism were cultivated 48 hours, and each test tube antibacterial of the centrifugal collection of difference, placed the 2ml normal saline, mixing, and it is the OD value at 540nm place that ultra-violet and visible spectrophotometer is surveyed wavelength.
1.3, toothpaste solution is to the influence of S.mutans acid production
Get the 3ml bacterial suspension inoculation respectively in the toothpaste solution of each concentration of equivalent, 37 ℃ of following anaerobism were cultivated 48 hours, and calculated the △ pH value before and after cultivating, and with the △ pH value contrast of negative control group.
1.4, toothpaste solution is to the influence of S.mutans adhesive attraction
Be the ratio of 10:1 in toothpaste solution and bacteria suspension, respectively with bacterial suspension inoculation in the toothpaste solution of each concentration, after 30 ° of horizontal angle anaerobism of all test tubes are cultivated 48h, with the antibacterial that adheres to test tube wall NaOH eluant solution, measure wavelength in the OD at 540nm place value, and calculate the adhesion inhibition rate, with the adhesion inhibition rate contrast of negative control group.
1.5, glucosyltransferase (Glucosyltransferase, the detection of extraction GTF) and water-insoluble extracellular polysaccharide (WIG)
Get each 3ml of toothpaste solution of variable concentrations, add S.mutans bacteria suspension 0.3ml, anaerobism is centrifugal with inoculum after cultivating, and collects supernatant, add solid ammonium sulfate, make saturation reach 60%, centrifugal after, precipitation is dissolved in the phosphate buffer dialyses, centrifugal, supernatant is the thick enzyme of GTF.Get the thick enzyme of 0.1mlGTF, add the 4ml distilled water, adopt Coomassie brilliant blue method (Bradford method) to measure total protein content.Other gets 100 μ l0.5mmol/L sucrose solutions, the thick enzyme 0.1ml of GTF, add the 0.1mmol/L sodium phosphate buffer, make the cumulative volume of mixed liquor reach 500 μ l, hatch 60min for 37 ℃, be heated to cessation reaction behind 100 ℃ of lasting 10min, add 2.5ml distilled water mixing, centrifugal, collect supernatant and adopt the Smogyi method to measure reducing sugar amount in the enzyme one substrate reactions liquid.GTF unit of activity (IU) is defined as (37 ℃ of reaction 1h per minutes discharge the required enzyme amount of 1 μ mol reducing sugar from sucrose) under the standard conditions, and calculates the ratio vigor of enzyme.
It is centrifugal to get inoculum, abandons supernatant, and taking precipitate adds the NaOH5ml of 0.5mol/L, centrifugal, get supernatant, add the dehydrated alcohol of its 3 times of volumes, centrifugal, precipitation is the water-insoluble extracellular polysaccharide that reaction generates, and measures the content of water-insoluble extracellular polysaccharide with anthrone method.Enzymatic activity and the contrast of insoluble extracellular polysaccharide with S.mutans in the negative control group.
2, experimental result:
2.1, in above-mentioned experiment, Streptococcus mutans growth is all arranged in the toothpaste solution, and along with the rising of glycosides content in the sweet tea extract and the reduction of sweet tea tannins content, the concentration of Streptococcus mutans increases in the solution.The OD value population mean of experimental group S.mutans is lower than negative control group (P<0.01), namely when glycosides content in the sweet tea extract 5~95% and the scope of sweet tea tannins 2~21% in the time, growth to Streptococcus mutans has inhibition, and its inhibition increases with the reduction of glycosides content and the increase of sweet tea tannins content.Concrete outcome sees Table 1.
Table 1 toothpaste solution is to the inhibiting OD value of Streptococcus mutans (X ± s)
2.2, all have difference between △ pH (pH variable quantity) population mean before and after the toothpaste solution experiments, glycosides content is 5% in sweet tea extract, sweet tea tannins content is 21% o'clock, the △ pH value variable quantity of S.mutans is minimum; Significantly be lower than negative control group △ pH (P<0.001) between the population mean of experimental group △ pH value.Specifically see Table 2.
The influence that table 2 toothpaste solution is sour to the Streptococcus mutans product (X ± s)
2.3, along with the rising of glycosides content in the sweet tea extract, the reduction of sweet tea tannins content, the adhesion inhibition rate also decreases.The population mean that experimental group adheres to the OD value of bacterium liquid significantly is lower than negative control group group (p<0.01), and concrete outcome sees Table 3.
The influence that table 3 toothpaste solution adheres to Streptococcus mutans (X ± s)
2.4, experimental group is to the influence of total protein, GTF enzyme activity, water-insoluble extracellular polysaccharide in the S.mutans enzyme liquid
2.4.1 along with glycosides content in the sweet tea extract raises, the reduction of sweet tea tannins content, the content of total protein reduces on the contrary in the S.mutans enzyme liquid.Total protein content is higher than the negative control group group on the contrary in the toothpaste solution of experimental group variable concentrations.Specifically see Table 4.
Table 4 toothpaste solution is to the influence of total protein content in the S.mutans enzyme liquid (X ± s)
2.4.2 along with glycosides content in the sweet tea extract raises, the reduction of sweet tea tannins content, the GTF activity of S.mutans raises gradually.The reducing sugar amount of negative control group, enzyme activity, than vigor all apparently higher than experimental group (p<0.001).Specifically see Table 5.
Table 5 toothpaste solution is to the influence of GTF among the S.mutans (X ± s)
2.4.3 along with glycosides content in the sweet tea extract raises, the reduction of sweet tea tannins content, the synthetic water-insoluble extracellular polysaccharide content of S.mutans is rising trend; The ability of the insoluble extracellular polysaccharide of negative control group S.mutans synthetic water is significantly higher than experimental group (p<0.001).Specifically see Table 6.
Table 6 toothpaste solution is to the influence of the insoluble extracellular polysaccharide of S.mutans synthetic water (X ± s)
Through above-mentioned experiment, glycosides content is proportionate and is negative correlativing relation with sweet tea tannins content in the GTF enzymatic activity of experimental group and the sweet tea extract, in toothpaste sweet tea extract content one regularly, to the inhibition of S.mutans along with glycosides content increases, sweet tea tannins content reduces and descends.
Claims (10)
1. contain the toothpaste of sweet tea extract, comprise sweeting agent, it is characterized in that: described sweeting agent is sweet tea extract, and it accounts for 0.2~2.5% of this toothpaste weight; The weight content of glycosides is 5~40% in the described sweet tea extract, and the weight content of sweet tea tannins is 2~21%.
2. the toothpaste that contains sweet tea extract according to claim 1, it is characterized in that: described sweet tea extract accounts for 2~2.5% of this toothpaste weight.
3. the toothpaste that contains sweet tea extract according to claim 2, it is characterized in that: described sweet tea extract accounts for 2.5% of this toothpaste weight.
4. according to each described toothpaste that contains sweet tea extract in the claim 1~3, it is characterized in that: the weight content of glycosides is 5~40% in the described sweet tea extract, and the weight content of sweet tea tannins is 7~21%.
5. according to each described toothpaste that contains sweet tea extract in the claim 1~3, it is characterized in that: the weight content of glycosides is 5~40% in the described sweet tea extract, and the weight content of sweet tea tannins is 15~21%.
6. according to each described toothpaste that contains sweet tea extract in the claim 1~3, it is characterized in that: the weight content of glycosides is 5~35% in the described sweet tea extract, and the weight content of sweet tea tannins is 16~21%.
7. according to each described toothpaste that contains sweet tea extract in the claim 1~3, it is characterized in that: the weight content of glycosides is 5~30% in the described sweet tea extract, and the weight content of sweet tea tannins is 17~21%.
8. according to each described toothpaste that contains sweet tea extract in the claim 1~3, it is characterized in that: the weight content of glycosides is 5~20% in the described sweet tea extract, and the weight content of sweet tea tannins is 18~21%.
9. according to each described toothpaste that contains sweet tea extract in the claim 1~3, it is characterized in that: the weight content of glycosides is 5~10% in the described sweet tea extract, and the weight content of sweet tea tannins is 18~21%.
10. according to each described toothpaste that contains sweet tea extract in the claim 1~3, it is characterized in that: the weight content of glycosides is 5% in the described sweet tea extract, and the weight content of sweet tea tannins is 21%.
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CN106377464A (en) * | 2016-11-21 | 2017-02-08 | 遵义医学院 | Application of Lithocarpus polystachyus (Wall.) Rehd. in preparing toothpaste |
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CN1308932A (en) * | 2001-01-05 | 2001-08-22 | 云南省农业科学院生物技术研究所 | Desensitizing toothpaste and its preparing process |
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Title |
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梁文红等: "茶多酚对变形链球菌的体外抗菌活性研究", 《遵义医学院学报》 * |
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CN106377464A (en) * | 2016-11-21 | 2017-02-08 | 遵义医学院 | Application of Lithocarpus polystachyus (Wall.) Rehd. in preparing toothpaste |
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