CN103007090A - Preparation and application of sugarcane leaf extractive for preventing and curing decsyed teeth and preparations - Google Patents
Preparation and application of sugarcane leaf extractive for preventing and curing decsyed teeth and preparations Download PDFInfo
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- CN103007090A CN103007090A CN2013100147849A CN201310014784A CN103007090A CN 103007090 A CN103007090 A CN 103007090A CN 2013100147849 A CN2013100147849 A CN 2013100147849A CN 201310014784 A CN201310014784 A CN 201310014784A CN 103007090 A CN103007090 A CN 103007090A
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- sacchari sinensis
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Abstract
The invention relates to a sugarcane leaf extractive for preventing and curing decsyed teeth, a preparation method of the sugarcane leaf extractive, preparation methods of different preparations and applications, which are characterized by comprising the sugarcane leaf extractive for preventing and curing decsyed teeth, an extraction process of the sugarcane leaf extractive, preparation of the sugarcane leaf extractive into products for preventing and curing decsyed teeth (comprising medicines, functional foods and chemical products) and applications of the products. According to the invention, the agricultural waste sugarcane leaves are used as the raw material; therefore, the sugarcane leaf extractive has the advantages of being free from toxic and side effects, low in cost, complete in process and exact in effect and is suitable for popularization and application.
Description
Technical field
The present invention relates to a kind of leaf of Caulis Sacchari sinensis extract and extraction process thereof be used to preventing and treating dental caries, also relate to the application of leaf of Caulis Sacchari sinensis extract in preparation medicine, functional food and chemical products.
Background technology
Caulis Sacchari sinensis (Saccharum sinensis Roxb.) is the perennial saccharum plant of grass family, extensively plants in 1600 meters with lower temperate zone and torrid areas.In recent years, China's Caulis Sacchari sinensis total output reaches more than one hundred million tons, and it is over half that wherein the Guangxi sugarcane yield accounts for the whole nation.Caulis Sacchari sinensis is with a long history in China plantation, and except being used for sugaring, China put down in writing according to Compendium of Material Medica with Caulis Sacchari sinensis juice, skin, the slag existing history of more than one thousand years of curing the disease: " sugarcane, the fruit of spleen also, its slurry is sweet trembles with fear, and the energy pathogenic fire purging is hot.", the traditional Chinese medical science thinks that this product sweet in the mouth is cool in nature, clearing away heat and promoting production of body fluid is arranged, moisturize the effect such as relieve the effect of alcohol, and can be used for the diseases such as calentura Tianjin wound, restlessness and thirst, regurgitation vomiting, xeropulmonary cough, constipation due to dry stool.China grows cane mainly for the production of sucrose, however the leaf of Caulis Sacchari sinensis that accounts for Caulis Sacchari sinensis 15% except part is used for animal feeding-stuff, all the other major parts are burned on the spot, not only contaminated environment but also waste resource.Studies show that leaf of Caulis Sacchari sinensis contains abundant chemical constituent, have important economic worth and widely pharmacological action, reconcile the pharmacologically actives such as immunity such as antibacterial, antioxidation, antitumor and resisting fatigue.The leaf of Caulis Sacchari sinensis aboundresources if further investigate and develop its medical value, not only makes the sugarcane grower obtain economic benefit, can also alleviate Chinese herbal medicine resource and lack problem, promotes the sustainable development of Chinese herbal medicine resource.
Summary of the invention
The object of the invention provides a kind of method of extracting the dental caries active component from leaf of Caulis Sacchari sinensis, the efficient isolation technics of extraction process utilization, and used filler macroporous adsorbent resin and polyamide all can circular regenerations.The invention solves the recycling of agricultural waste material leaf of Caulis Sacchari sinensis, avoided having the waste of medical value leaf of Caulis Sacchari sinensis.
The inventor is by the research to leaf of Caulis Sacchari sinensis, find that leaf of Caulis Sacchari sinensis separates the extract that obtains through the inventive method and has obvious dental caries effect, the test of pesticide effectiveness studies show that leaf of Caulis Sacchari sinensis extract of the present invention all has obvious inhibitory action to causing dental caries Streptococcus mutans and actinomyces viscosus in the oral cavity.
Leaf of Caulis Sacchari sinensis extract among the present invention, its preparation method is as follows:
1, preparation method:
(1) preparation method one
Get leaf of Caulis Sacchari sinensis, clean, dry, pulverizing are extracted, are concentrated through routine, concentrated solution at first take water or moisture lower alcohol as eluant on the polyamide column eluting, take anhydrous or moisture lower alcohol as eluant, get alcohol eluen again, the eluent concentrating under reduced pressure, drying gets the leaf of Caulis Sacchari sinensis extract.
The preparation method explanation:
Described conventional extracting method includes but not limited to that flooding, decocting boil, pure lixiviate, alcohol reflux are extracted, alcohol percolation.
Described conventional method for concentration includes but not limited to that normal pressure is concentrated, concentrating under reduced pressure, reverse osmosis concentration.
Described drying includes but not limited to spray drying, lyophilization.
Preferably, when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
Preferably, as the second time eluant lower alcohol be ethanol; More excellent, lower alcohol is ethanol; Best, described lower alcohol be ethanol and as the second time eluant concentration be 30～100% ethanol.
(2) preparation method two
Get leaf of Caulis Sacchari sinensis, clean, dry, pulverize, through routine extract, concentrated, concentrated solution at first take water or moisture lower alcohol as eluant on the polyamide column eluting, take anhydrous or moisture lower alcohol as eluant, get alcohol eluen again, eluent is concentrated; Afterwards, concentrated solution is gone up polyamide column at first take water or moisture lower alcohol as eluant, take anhydrous or moisture lower alcohol as eluant, gets alcohol eluen again, and eluent is concentrated, and drying gets the leaf of Caulis Sacchari sinensis extract.
The preparation method explanation:
Described conventional extracting method includes but not limited to that flooding, decocting boil, pure lixiviate, alcohol reflux are extracted, alcohol percolation.
Described conventional method for concentration includes but not limited to that normal pressure is concentrated, concentrating under reduced pressure, reverse osmosis concentration.
Described drying includes but not limited to spray drying, lyophilization.
Preferably, for last polyamide column, when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
Preferably, for last polyamide column, the lower alcohol of eluant is ethanol as the second time; More excellent, lower alcohol is ethanol; Best, described lower alcohol be ethanol and as the second time eluant concentration be 30～100% ethanol.
(3) preparation method three
Get leaf of Caulis Sacchari sinensis, clean, dry, pulverize, through routine extract, concentrated, concentrated solution at first take water or moisture lower alcohol as eluant on the macroporous adsorptive resins eluting, take anhydrous or moisture lower alcohol as eluant, get alcohol eluen again, eluent is concentrated; Afterwards, concentrated solution is gone up polyamide column at first take water or moisture lower alcohol as eluant, take anhydrous or moisture lower alcohol as eluant, gets alcohol eluen again, and eluent is concentrated, and drying gets the leaf of Caulis Sacchari sinensis extract.
The preparation method explanation:
Described conventional extracting method includes but not limited to that flooding, decocting boil, pure lixiviate, alcohol reflux are extracted, alcohol percolation.
Described conventional method for concentration includes but not limited to that normal pressure is concentrated, concentrating under reduced pressure, reverse osmosis concentration.
Described drying includes but not limited to spray drying, lyophilization.
Preferably, macroporous adsorptive resins is AB-8.
Preferably, for upper macroporous adsorptive resins, when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
Preferably, for upper macroporous adsorptive resins, the lower alcohol of eluant is ethanol as the second time; More excellent, lower alcohol is ethanol; Best, described lower alcohol be ethanol and as the second time eluant concentration be 10～70% ethanol.
Preferably, for upper polyamide column, when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
Preferably, for upper polyamide column, the lower alcohol of eluant is ethanol as the second time; More excellent, lower alcohol is ethanol; Best, described lower alcohol be ethanol and as the second time eluant concentration be 30～100% ethanol.
(4) preparation method four.
Get leaf of Caulis Sacchari sinensis, clean, dry, pulverize, through routine extract, concentrated, concentrated solution at first take water or moisture lower alcohol as eluant on the polyamide column eluting, take anhydrous or moisture lower alcohol as eluant, get alcohol eluen again, eluent is concentrated; Afterwards, concentrated solution is gone up macroporous adsorptive resins at first take water or moisture lower alcohol as eluant, take anhydrous or moisture lower alcohol as eluant, gets alcohol eluen again, and eluent is concentrated, and drying gets the leaf of Caulis Sacchari sinensis extract.
The preparation method explanation:
Described conventional extracting method includes but not limited to that flooding, decocting boil, pure lixiviate, alcohol reflux are extracted, alcohol percolation.
Described conventional method for concentration includes but not limited to that normal pressure is concentrated, concentrating under reduced pressure, reverse osmosis concentration.
Described drying includes but not limited to spray drying, lyophilization.
Preferably, for upper polyamide column, when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
Preferably, for upper polyamide column, the lower alcohol of eluant is ethanol as the second time; More excellent, lower alcohol is ethanol; Best, described lower alcohol be ethanol and as the second time eluant concentration be 30～100% ethanol.
Preferably, macroporous adsorptive resins is AB-8.
Preferably, for upper macroporous adsorptive resins, when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
Preferably, for upper macroporous adsorptive resins, the lower alcohol of eluant is ethanol as the second time; More excellent, lower alcohol is ethanol; Best, described lower alcohol be ethanol and as the second time eluant concentration be 10～70% ethanol.
2, some preparation method embodiment of leaf of Caulis Sacchari sinensis extract:
Embodiment 1
Extraction process: get leaf of Caulis Sacchari sinensis, clean, dry, pulverizing, with 70% ethanol water reflux, extract, secondary, solid-liquid ratio is 1: 8～1: 10, extracts 80 ℃ of temperature, extracts 2h at every turn, and merge extractive liquid, filters, and filtrate is concentrated into nothing alcohol and distinguishes the flavor of; The concentrated solution defat with petroleum ether until petroleum ether portion is colourless, continues to concentrate to get leaf of Caulis Sacchari sinensis extractum.
Separating technology: leaf of Caulis Sacchari sinensis extractum adds an amount of distilled water diluting, is splined on the good polyamide column of handling well of pretreatment, uses first the distilled water eluting of 3 times of column volumes; Second step is with the ethanol elutions of 10 times of amount column volume 30%-70%; The 3rd step got alcohol eluen with 5 times of amount column volume 95% ethanol elutions, and drying obtains the leaf of Caulis Sacchari sinensis extract.
Embodiment 2
Extraction process: get leaf of Caulis Sacchari sinensis, clean, dry, pulverizing, with 70% ethanol water reflux, extract, secondary, solid-liquid ratio is 1: 8～1: 10, extracts 80 ℃ of temperature, extracts 2h at every turn, and merge extractive liquid, filters, and filtrate is concentrated into nothing alcohol and distinguishes the flavor of; The concentrated solution defat with petroleum ether until petroleum ether portion is colourless, continues to concentrate to get leaf of Caulis Sacchari sinensis extractum.
Separating technology: leaf of Caulis Sacchari sinensis extractum adds an amount of distilled water diluting, be splined on the good polyamide column of pretreatment, use first the water elution of 3 times of column volumes, use again 70% ethanol elution of 10 times of column volumes, collect and merge 70% ethanol elution, concentration and recovery solvent to 1/10 volume; 70% eluting concentrated solution is splined on the good polyamide column of pretreatment, at first uses the distilled water eluting of 3 times of column volumes; Second step is with the ethanol elutions of 10 times of amount column volume 30%-70%; The 3rd step got alcohol eluen with 5 times of amount column volume 95% ethanol elutions, and drying obtains the leaf of Caulis Sacchari sinensis extract.
Embodiment 3
Extraction process: get leaf of Caulis Sacchari sinensis, clean, dry, pulverizing, with 70% ethanol water reflux, extract, secondary, solid-liquid ratio is 1: 8～1: 10, extracts 80 ℃ of temperature, extracts 2h at every turn, and merge extractive liquid, filters, and filtrate is concentrated into nothing alcohol and distinguishes the flavor of; The concentrated solution defat with petroleum ether until petroleum ether portion is colourless, continues to concentrate to get leaf of Caulis Sacchari sinensis extractum.
Separating technology: leaf of Caulis Sacchari sinensis extractum adds an amount of distilled water diluting, be splined on the good AB-8 macroporous adsorptive resins of pretreatment, use first the water elution of 3 times of column volumes, use again 5 times of column volume 10% ethanol elutions, use at last 70% ethanol elution of 3 times of column volumes, collect and merge 70% ethanol elution, concentration and recovery solvent to 1/10 volume; Leaf of Caulis Sacchari sinensis macroporous adsorbent resin 70% eluting concentrated solution is splined on the good polyamide column of pretreatment, at first uses the distilled water eluting of 3 times of column volumes; Second step is with the ethanol elutions of 10 times of amount column volume 30%-70%; The 3rd step got alcohol eluen with 5 times of amount column volume 95% ethanol elutions, and drying obtains the leaf of Caulis Sacchari sinensis extract.
Embodiment 4
Extraction process: get leaf of Caulis Sacchari sinensis, clean, dry, pulverizing, with 70% ethanol water reflux, extract, secondary, solid-liquid ratio is 1: 8～1: 10, extracts 80 ℃ of temperature, extracts 2h at every turn, and merge extractive liquid, filters, and filtrate is concentrated into nothing alcohol and distinguishes the flavor of; The concentrated solution defat with petroleum ether until petroleum ether portion is colourless, continues to concentrate to get leaf of Caulis Sacchari sinensis extractum.
Separating technology: leaf of Caulis Sacchari sinensis extractum adds an amount of distilled water diluting, is splined on the good polyamide column of pretreatment, at first uses the distilled water eluting of 3 times of column volumes; Second step is with the ethanol elutions of 10 times of amount column volume 30%-70%; The 3rd step got alcohol eluen, concentration and recovery solvent to 1/10 volume with 5 times of amount column volume 95% ethanol elutions; Concentrated solution is splined on the good AB-8 macroporous adsorptive resins of pretreatment, uses first the water elution of 3 times of column volumes, uses 5 times of column volume 10% ethanol elutions again, use at last 70% ethanol elution of 3 times of column volumes, collect merging 70% ethanol elution, drying obtains the leaf of Caulis Sacchari sinensis extract.
The different preparations of leaf of Caulis Sacchari sinensis extract among the present invention, its preparation method is as follows:
1, preparation method:
Get the leaf of Caulis Sacchari sinensis extract that above-mentioned preparation method makes, add according to a conventional method adjuvant, make different preparations.
2, some dosage form preparation method embodiment of the different preparations of leaf of Caulis Sacchari sinensis extract:
The preparation of embodiment 1 leaf of Caulis Sacchari sinensis dental caries buccal tablet
The leaf of Caulis Sacchari sinensis extract with excipient, correctives, binding agent mixing, with granulator granulation and dry granulation, is added lubricant again, be shaped with the tablet machine tabletting, tablet is sent into seed-coating machine and is carried out the polishing coating, namely gets leaf of Caulis Sacchari sinensis dental caries buccal tablet.
The preparation of embodiment 2 leaf of Caulis Sacchari sinensis dental caries chewing gum
With gel matrix melting under 45 ℃-60 ℃ temperature, add together abundant stirring and evenly mixing of emulsifying agent, correctives, wetting agent, when treating that temperature drops to 40 ℃, add again leaf of Caulis Sacchari sinensis extract stirring and evenly mixing, enter mould, tabletting, section, molding, namely get leaf of Caulis Sacchari sinensis dental caries chewing gum.
The preparation of embodiment 3 leaf of Caulis Sacchari sinensis dental caries buccal drop pills
With excipient, correctives, binding agent mixing, with granulator granulation and dry granulation, drying adds in the substrate of melting with the leaf of Caulis Sacchari sinensis extract; stir evenly, splash in the condensing agent, take out drop pill; the eccysis condensing agent, drying namely gets leaf of Caulis Sacchari sinensis dental caries buccal drop pills.
The preparation of embodiment 4 leaf of Caulis Sacchari sinensis anti-caries oral effervescent tablets
The leaf of Caulis Sacchari sinensis extract with filler, correctives, binding agent mixing, with granulator granulation and dry granulation, is added lubricant again, be shaped with the tablet machine tabletting, tablet is sent into seed-coating machine and is carried out the polishing coating, namely gets leaf of Caulis Sacchari sinensis anti-caries oral effervescent tablet.
The preparation of embodiment 5 leaf of Caulis Sacchari sinensis dental caries toothpaste
The leaf of Caulis Sacchari sinensis extract is mixed with wetting agent, water, glucide, sodium dihydrogen phosphate, pigment, thickening agent, abrasivus, foaming agent and essence, and it is also degassed to stir, and makes mastic, and packing namely gets leaf of Caulis Sacchari sinensis dental caries toothpaste.
Pharmacology embodiment:
Streptococcus mutans and actinomyces viscosus are inoculated in the BHI culture fluid, place the anaerobism culture bag, in 37 ℃ of constant temperature culture 18h, under 722 spectrophotometers, than turbid, transfer OD550nm value to 1.0 with normal saline, for subsequent use.
With aseptic brain-heart infusion medium (BHI) doubling dilution the leaf of Caulis Sacchari sinensis extract is prepared into 16mg/ml, 8mg/ml, 4mg/ml, 2mg/ml, 1mg/ml, 0.5mg/ml, the drug dilution liquid of 0.25mg/ml.In 1: 1 ratio, each 100 μ l was inoculated in respectively 96 orifice plates, sets up simultaneously solvent control group (DMSO) with the Streptococcus mutans that prepared and actinomyces viscosus bacterial suspension and each group medicinal liquid, behind oscillator concussion 1min, put into the anaerobism bag in 80%N2,20%CO2,37 ℃ of constant temperature culture 24H.In the culture fluid without the minimum diluted concentration of bacterial growth as minimum inhibitory concentration (MIC).
Choose administration concentration greater than each hole of MIC, get respectively 20 μ l and coat on the BHI solid medium, cultivate 24H under the same terms, it is minimum bactericidal concentration (MBC) that the observation clump count is less than the individual least concentration of 5-6.
Experimental result shows that the leaf of Caulis Sacchari sinensis extract is 1mg/ml to Streptococcus mutans and actinomyces viscosus minimum inhibitory concentration (MIC).Minimum bactericidal concentration (MBC) is 4mg/ml.
This experimentation confirms that multiple effective antipathogenic composition is arranged in the leaf of Caulis Sacchari sinensis, and the common caries bacteria that causes in oral cavity is all had inhibitory action, and the leaf of Caulis Sacchari sinensis extract is antibacterial suitable with the tea polyphenols effect with bactericidal effect to Streptococcus mutans and actinomyces viscosus.
Claims (12)
1. the application of medicine, functional food and the chemical products of the preparation of a leaf of Caulis Sacchari sinensis extract and conduct prevention thereof and treatment dental caries, wherein said leaf of Caulis Sacchari sinensis extract prepares by the following method: leaf of Caulis Sacchari sinensis is pulverized, take water or lower alcohol as solvent, extract, concentrate, separate with the polyamide post through macroporous resin column, collect eluent, obtain the leaf of Caulis Sacchari sinensis extract after the drying.Contain polysaccharide 2-10% in this extract, total flavones 1-2%.
2. by leaf of Caulis Sacchari sinensis extract claimed in claim 1, it is characterized in that the step of described upper polyamide column is: (1) is take water or moisture lower alcohol as eluant upper prop eluting; (2) take anhydrous or moisture lower alcohol as eluant, get alcohol eluen.
3. by leaf of Caulis Sacchari sinensis extract claimed in claim 1, it is characterized in that separating step also is included in the before upper macroporous adsorptive resins of polyamide column on the extracting solution.
4. by leaf of Caulis Sacchari sinensis extract claimed in claim 1, it is characterized in that separating step also is included in and goes up macroporous adsorptive resins or polyamide column on the extracting solution after the polyamide column again.
5. by claim 3 or 4 described leaf of Caulis Sacchari sinensis extracts, it is characterized in that the step of upper macroporous adsorbent resin is: (1) is take water or moisture lower alcohol as eluant upper prop eluting; (2) take anhydrous or moisture lower alcohol as eluant, get alcohol eluen.
6. by leaf of Caulis Sacchari sinensis extract claimed in claim 1, it is characterized in that when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
7. by leaf of Caulis Sacchari sinensis extract claimed in claim 1, it is characterized in that the lower alcohol of eluant is ethanol as the second time.
8. by leaf of Caulis Sacchari sinensis extract claimed in claim 7, it is characterized in that described concentration of alcohol is 30～100%.
9. by leaf of Caulis Sacchari sinensis extract claimed in claim 5, it is characterized in that described macroporous adsorbent resin is AB-8.
10. by leaf of Caulis Sacchari sinensis extract claimed in claim 5, it is characterized in that when eluant all adopted moisture lower alcohol, the concentration of lower alcohol of eluant was lower than as the concentration of the lower alcohol of eluant for the second time as the first time.
11. by leaf of Caulis Sacchari sinensis extract claimed in claim 5, it is characterized in that the lower alcohol of eluant is ethanol as the second time.
12. by the described leaf of Caulis Sacchari sinensis extract of claim 11, it is characterized in that described concentration of alcohol is 10～100%.
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| CN104306758A (en) * | 2014-09-28 | 2015-01-28 | 广西大学 | Method for extracting polyphenol from sugar cane bark |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104306758A (en) * | 2014-09-28 | 2015-01-28 | 广西大学 | Method for extracting polyphenol from sugar cane bark |
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| CN112137940B (en) * | 2019-06-26 | 2022-11-15 | 广西中医药大学 | Compound sugarcane leaf toothpaste and preparation method thereof |
| CN114209638A (en) * | 2021-12-31 | 2022-03-22 | 广西养利农业投资开发有限公司 | Compound broadleaf holly leaf traditional Chinese medicine composition for preparing toothpaste and compound broadleaf holly leaf traditional Chinese medicine toothpaste |
| CN114209638B (en) * | 2021-12-31 | 2023-07-14 | 广西养利农业投资开发有限公司 | Compound kuding tea traditional Chinese medicine composition for preparing toothpaste and compound kuding tea traditional Chinese medicine toothpaste |
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Application publication date: 20130403 |