CN100581534C - Galangal rhizome extract preparation process - Google Patents
Galangal rhizome extract preparation process Download PDFInfo
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- CN100581534C CN100581534C CN200610124034A CN200610124034A CN100581534C CN 100581534 C CN100581534 C CN 100581534C CN 200610124034 A CN200610124034 A CN 200610124034A CN 200610124034 A CN200610124034 A CN 200610124034A CN 100581534 C CN100581534 C CN 100581534C
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Abstract
The present invention is oral hygiene composite with galangal rhizome extract and its preparation process. The galangal rhizome extract contains galangin in 1-25 % and total flavone over 10 %, and has been treated to eliminate its pungency and color. The galangal rhizome extract has enriched the active antiseptic, antiphlogistic, antiviral and analgesic components of galangal rhizome, less pungency oil component and low chroma, and is suitable for use in oral hygiene composite. The oral hygiene composite is safe, reliable, low in cost and acceptable.
Description
Technical field
The present invention relates to natural plant extracts, particularly Rhizoma Alpiniae Officinarum extract and preparation method thereof and be the oral hygiene composition of active component with the Rhizoma Alpiniae Officinarum extract.
Background technology
Zingiberaceae Alpinia plants Rhizoma Alpiniae Officinarum (Alpinia officinarum Hance) has long use and medicinal history in China, has the effect of warming middle-JIAO, cold expelling, pain relieving, spasmolytic, is used for the treatment of coldness and pain in the epigastrium, vomiting, toothache etc.
Rhizoma Alpiniae Officinarum is used for the treatment and the existing history of more than one thousand years of health care of oral disease as compound Chinese herbal medicinal ingredients.Compendium of Material Medica have " with two cun of Rhizoma Alpiniae Officinarums, one piece of Scorpio (roasting), be ground into the end, chafe the place, the saliva that spues is gargled with salt soup " treat wind have a toothache bullate record (referring to Li Shizhen (1518-1593 A.D.). Compendium of Materia Medica, careless portion); Chinese patent " a kind of Chinese medicine preparation for the treatment of toothache and preparation method thereof " (patent No. ZL 97105163.1) and " a kind of Chinese powder medicine for the treatment of toothache " (ZL 200410055504.X) disclose Rhizoma Alpiniae Officinarum is used for oral disease therapeutic and health care as compound Chinese herbal medicinal ingredients technical scheme.
Modern pharmacology studies show that, flavonoid chemical constituents such as galangin contained in the Rhizoma Alpiniae Officinarum have antibiotic, antiinflammatory, antiviral and analgesic activity: document " native chemical composition galangin progress ", people such as He Rui, " time precious traditional Chinese medical science traditional Chinese medicines " magazine, 1999 the 10th the 10th phases of volume, 788-789 page or leaf report, from Chinese medicine Rhizoma Alpiniae Officinarum (Alpinia officinarum Hance) rhizome, galangin (the galangin that extraction separation goes out in the aerial parts of South Africa plant Helichrysum aureonitens and a plurality of geographic propolis, 3,5, the 7-trihydroxyflavone), be proved to be have antibiotic, antiinflammatory and antivirus action; Document " pharmacodynamic study of galangin ", people such as Wu Qinghe, " Chinese crude drug " magazine, volume o. 11th, 699-700 page or leaf reported that the active component that Rhizoma Alpiniae Officinarum plays analgesic activity was flavone compounds such as galangin and kaempferol in 2000 the 23rd.
Existing propolis extract oral hygiene composition emerges, as propolis extract toothpaste.Contain flavonoid active component such as galangin in the propolis extract, but propolis contains the sensitization source.Document " biologic activity of propolis and toxicity and anaphylaxis ", people such as Hu Fuliang, " science and technology circular " magazine, 2003 19 the 2nd phases of volume, the 168th page of report, propolis is applied on cosmetics, the toothpaste, has caused the hypersensitive increase of propolis.And, only more than 400 ton of the annual production of China's propolis, resource is deficient to be lacked, costs an arm and a leg.
Rhizoma Alpiniae Officinarum is rich in flavones ingredients such as galangin, but does not see that as yet Rhizoma Alpiniae Officinarum extract is applied in the oral hygiene composition.
Need allow people will be appreciated that, exploitation Rhizoma Alpiniae Officinarum medicine resource, the Rhizoma Alpiniae Officinarum extract that will contain flavonoid active component such as galangin are applied to oral hygiene composition, can promote the well-being of mankind, have remarkable economical and social meaning: Rhizoma Alpiniae Officinarum is rich in that flavonoids such as galangin are antibiotic, antiinflammatory, antiviral and analgesic bioactive substance; Rhizoma Alpiniae Officinarum is used for existing thousand history of the treatment of oral disease and health care, is the dual-purpose natural plants of medicated diet, and is safe and harmless, contains the sensitization source unlike propolis; That Rhizoma Alpiniae Officinarum is widely planted, originated is abundant, price is more cheap than propolis; Yet flavonoid active component content such as galangin is low in the Rhizoma Alpiniae Officinarum extract that conventional extracting method obtains, and mouthfeel is too pungent, color is dark too, therefore is used to prepare oral hygiene composition and is not accepted by masses, need do technological improvement.
Summary of the invention
The object of the present invention is to provide a kind of Rhizoma Alpiniae Officinarum extract and preparation method thereof, adopt to extract flavonoid active component such as galangin in the enrichment Rhizoma Alpiniae Officinarum, remove most of pungent volatile oil component in the Rhizoma Alpiniae Officinarum, and the preparation method of decolouring, make Rhizoma Alpiniae Officinarum extract be rich in flavonoid active component such as galangin, significantly reduce the acid and the colourity of Rhizoma Alpiniae Officinarum extract.
Another object of the present invention is that the Rhizoma Alpiniae Officinarum extract that will contain flavonoid active component such as galangin is applied in the oral hygiene composition.
The object of the present invention is achieved like this: a kind of Rhizoma Alpiniae Officinarum extract is characterized in that: count by weight percentage, the galangin content in the described Rhizoma Alpiniae Officinarum extract 1～25%, general flavone content＞10%.
The preparation method of above-mentioned Rhizoma Alpiniae Officinarum extract, it is characterized in that comprising following sequential steps: carry out solvent extraction after the Rhizoma Alpiniae Officinarum dry rhizome is pulverized, add ethanol in extracting solution and make aquiferous ethanol solution, in this aquiferous ethanol solution, add petroleum ether, extraction, layering, divide then and get the aquiferous ethanol solution layer, add active carbon reflux decolouring after-filtration, reclaim ethanol and be concentrated into driedly, obtain above-mentioned Rhizoma Alpiniae Officinarum extract.
A kind of oral hygiene composition contains above-mentioned Rhizoma Alpiniae Officinarum extract.
This oral hygiene composition with galangal rhizome extract comprises the conventional ingredient of oral hygiene composition, it is characterized in that: press the final composition percentage by weight and calculate, also comprise 0.05～5% above-mentioned Rhizoma Alpiniae Officinarum extract in the compositions.
Above-mentioned oral hygiene composition with galangal rhizome extract can be toothpaste, tooth gel, collutory, tablet, dentifrice or chewing gum or the like." conventional ingredient of oral hygiene composition " of the present invention comprises conventional component well known in the art in toothpaste, tooth gel, collutory, tablet, dentifrice or the chewing gum.These conventional components can be other chemical compound of the carrier, additive and some properties that suit, for example grinding agent, surfactant, wetting agent, binding agent, thickening agent, correctives, coloring agent, antiseptic, solvent and fluorine source or the like.
Rhizoma Alpiniae Officinarum extract preparation method of the present invention has adopted aquiferous ethanol-petroleum ether solvent extract and separate scheme, utilize flavonoid active component such as galangin at aquiferous ethanol phase partition coefficient height and volatile oil component in the high characteristics of petroleum ether phase partition coefficient, enrichment flavonoid active component such as galangin, removed most of pungent volatile oil component in the Rhizoma Alpiniae Officinarum.
Oral hygiene composition with galangal rhizome extract of the present invention is owing to added the Rhizoma Alpiniae Officinarum extract that contains flavonoid active component such as galangin, when these compositionss are applied to the oral cavity, flavonoid active component such as galangin can bring into play that it is antibiotic, antiinflammatory, antiviral and analgesic activity, for prevention and treatment human body diseases bring beneficial effect, thereby has the health care effect.Described human body diseases can be the oral cavity partial disease, the disease that causes because of antibacterial, virus, inflammation or pain as periodontitis, gingivitis, oral ulcer or halitosis etc.; Also can be because of antibacterial or the viral disease that causes via the oral cavity route importing, as viral infection, bacterial infection, influenza, pharyngolaryngitis, gastropathy or intestinal tract disease etc.
The advantage that the present invention program had is:
1. the preparation method that adopted extract and enrichment antibiotic, the antiinflammatory of flavonoid such as galangin, antiviral and analgesic bioactive substance in the Rhizoma Alpiniae Officinarum.This Rhizoma Alpiniae Officinarum extract is applied to oral hygiene composition, but development and utilization Rhizoma Alpiniae Officinarum medicine resource, promotes the well-being of mankind, have remarkable economical and social meaning;
2. the preparation method that is adopted has been removed most of pungent volatile oil component in the Rhizoma Alpiniae Officinarum, the acid of gained Rhizoma Alpiniae Officinarum extract has obtained remarkable reduction, the oral hygiene composition with galangal rhizome extract of preparing has light Rhizoma Alpiniae Officinarum fragranced, is easily accepted by popular;
3. the preparation method that is adopted significantly reduces the colourity of Rhizoma Alpiniae Officinarum extract, and the background color and luster of the oral hygiene composition with galangal rhizome extract of preparing is light, is easily accepted by popular;
4. the active component that resulting oral hygiene composition adds is had the food and medicament dual-purpose plant Rhizoma Alpiniae Officinarum of medicinal history in thousand, safe and reliable, no sensitization source by oneself;
5. Rhizoma Alpiniae Officinarum is rich in flavones ingredients such as galangin, and it is abundant widely to plant, originate, thereby resulting oral hygiene composition with galangal rhizome extract relative low price.
The specific embodiment
The present invention is described in further detail below by embodiment, but the present invention is not limited to this specific examples.
Embodiment 1: the preparation of Rhizoma Alpiniae Officinarum extract
1.0kg is crushed to 40 orders with the Rhizoma Alpiniae Officinarum dry rhizome, is extractant with the ethyl acetate, heating in water bath reflux, extract, 2h; Leach extracting solution, reclaim ethyl acetate after do not have the ester flavor, obtain 81.5g sepia thickness paste crude extract A; It is dissolved in ethanol, and making ethanol content is the aquiferous ethanol solution of 72% (v/v), adds isopyknic petroleum ether (60～90 ℃ of boiling ranges), extraction, layering in this aquiferous ethanol solution; Divide and to get the aquiferous ethanol solution layer, add active carbon reflux decolouring 30min, the filtration of 1% (w/w), decolouring filtrate＜65 ℃ ,-reclaim ethanol under the 0.095MPa condition and be concentrated into dried, yellow Rhizoma Alpiniae Officinarum extract B70.5g.
Flavones ingredient comprises galangin and kaempferol, kaempferol, Quercetin, isorhamnetin etc.
The content assaying method of galangin in the Rhizoma Alpiniae Officinarum extract: adopting reversed-phase high-performance liquid chromatography, is standard with the galangin, external standard method.HPLC condition: C
18Chromatographic column, mobile phase are 0.5% phosphate aqueous solution that contains 58% methanol, and UV-detector detects wavelength 267nm, 35 ℃ of column temperatures, flow velocity 1.0mL/min.
Content of total flavone assay method in the Rhizoma Alpiniae Officinarum extract: adopting polyamide column chromatography to separate, is eluent with 95% ethanol; Eluent is that developing solvent launches with toluene-ethyl acetate-formic acid (14: 4: 1) on silica gel g thin-layer plate, sprays 5% aluminum chloride alcoholic solution, detects flavone fluorescence speckle under the 365nm ultraviolet light, and collecting, merging the eluent that is detected flavone is test solution; Adopting ultraviolet spectrophotometry, is to detect wavelength with 360nm, is reference substance drawing standard curve with the rutin, measures the absorbance of test solution, content of total flavone in the calculation sample.
After testing, the content of galangin is 0.97% in this Rhizoma Alpiniae Officinarum raw material, and content of total flavone is 7.5%.The content of galangin is 11.8% in the extract that obtains, and content of total flavone is 81%.
Flavones ingredients such as galangin that contains in the Rhizoma Alpiniae Officinarum extract and kaempferol, kaempferol, Quercetin, isorhamnetin all have certain antibiotic, antiinflammatory, antiviral and analgesic activities:
Adopt chemoluminescence method to detect galangin to the chemiluminescent inhibitory action of neutrophil cell, the galangin of 0.27mg/mL is 73% to the suppression ratio of neutrophil cell chemiluminescence intensity, shows that galangin has very strong anti-inflammatory activity;
Galangin is respectively 0.5,0.5,0.1 to the minimal inhibitory concentration MIC (mg/mL) of staphylococcus aureus (Staphylococcus aureus), bacillus subtilis (Bacillussubtilis), Bacillus cercus (Bacillus cereus);
The galangin of 12 μ g/mL can significantly suppress herpes simplex virus HSV-1; The galangin of 47 μ g/mL can significantly suppress Coxsackie virus Cox.B1;
Adopt acetic acid to cause the analgesic activity of mouse writhing method and mice formaldehyde injury method evaluation galangin, the mice oral dose is that the galangin of 0.10g/kg body weight can have significant analgesia role.
The color contrast experiment:
Adopt optical colorimetry to do the colourity contrast experiment.Get 95% alcoholic solution A1 and the B1 that Rhizoma Alpiniae Officinarum crude extract A in the said extracted thing preparation experiment and Rhizoma Alpiniae Officinarum extract B make 1.0mg/ml respectively, A1 was carried out 1: 2 as solvent with 95% ethanol, 1: 4,～1: 64 serial proportional diluted, and with B1 contrast colourity, colorimetric is all carried out in color comparison tube.As a result, the A1 colourity of the colourity of B1 and 1: 32 is suitable.
The evaluation of mouthfeel:
(1) the pungent mouthfeel valve of the aqueous suspension of Rhizoma Alpiniae Officinarum crude extract A concentration detects
Getting Rhizoma Alpiniae Officinarum crude extract A, is solvent with water, is made into the aqueous suspension that concentration is 100mg/ml; Be solvent with water then, it carried out 1: 2 that 1: 4,1: 8～1: 1024 serial proportional diluted allowed 10 volunteers taste mouthfeel from the low concentration to the high concentration.Write down everyone and experience pungent valve concentration.
Rhizoma Alpiniae Officinarum crude extract A aqueous suspension valve concentration detects table
| Volunteer's numbering | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Extension rate | 256 | 128 | 256 | 256 | 128 | 256 | 256 | 512 | 512 | 128 |
| Concentration (mg/ml) | 0.39 | 0.78 | 0.39 | 0.39 | 0.78 | 0.39 | 0.39 | 0.20 | 0.20 | 0.78 |
Average valve concentration is 0.47mg/ml.
(2) the pungent mouthfeel valve of the aqueous suspension of Rhizoma Alpiniae Officinarum extract B concentration detects
Getting Rhizoma Alpiniae Officinarum extract B, is solvent with water, is made into the aqueous suspension that concentration is 1.00g/ml; Be solvent with water then, it carried out 1: 2 that 1: 4,1: 8～1: 128 serial proportional diluted allowed 10 volunteers taste mouthfeel from the low concentration to the high concentration.Write down everyone and experience pungent valve concentration.
The valve concentration of Rhizoma Alpiniae Officinarum extract B aqueous suspension detects (n=10)
| Volunteer's numbering | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Extension rate | 16 | 32 | 16 | 16 | 16 | 16 | 16 | 32 | 16 | 16 |
| Concentration (mg/ml) | 62.5 | 31.2 | 62.5 | 62.5 | 62.5 | 62.5 | 62.5 | 31.2 | 62.5 | 62.5 |
Average valve concentration is 56.2mg/ml.
The valve concentration of Rhizoma Alpiniae Officinarum crude extract A is 0.47mg/ml, and the average valve concentration of Rhizoma Alpiniae Officinarum extract B is 56.2mg/ml, shows that Rhizoma Alpiniae Officinarum extract B acid greatly reduces.
Embodiment 2: toothpaste (Wt%) and preparation method
Prescription: glycerol 29, carboxymethyl cellulose (CMC) 0.6, hydroxyethyl-cellulose (HEC) 0.5, glucide 0.35, benzoic acid 0.15, calcium hydrogen phosphate 49～51, sodium lauryl sulfate 2.6, Rhizoma Alpiniae Officinarum extract 0.45, water surplus, and make that each constituent content percent sum equals 100% in the compositions.
Preparation method: by prescription, glucide, benzoic acid are dissolved in the water, Rhizoma Alpiniae Officinarum extract, CMC, HEC are dispersed in the glycerol, both mix homogeneously add calcium bicarbonate and sodium lauryl sulfate, mixed grinding, kneading, and vacuum outgas, canned.The toothpaste that obtains is beautiful white, has light Rhizoma Alpiniae Officinarum fragranced.
Embodiment 3: tooth gel prescription (Wt%) and preparation method
Prescription: glycerol 8.0, carbomer 5.0, propylene glycol 60, Rhizoma Alpiniae Officinarum extract 4.0 is regulated pH value with a small amount of diethanolamine, water surplus, and make that each constituent content percent sum equals 100% in the compositions.
Preparation method: by prescription, get glycerol and put in the mortar, add carbomer and fully grind, make it moistening, again with propylene glycol, Rhizoma Alpiniae Officinarum extract adds fully grinding in the above-mentioned mortar; Adding distil water is while stirring regulated pH to neutral then, makes it to form gel, and centrifugal removal bubble gets final product.Obtain tooth gel and be jade green, have light Rhizoma Alpiniae Officinarum fragranced.
Embodiment 4: collutory prescription (Wt%) and preparation method
Prescription: Rhizoma Alpiniae Officinarum extract 0.05～5.0, glucide 0.25～0.3, sodium monofluorophosphate 0.5～1.0, benzoic acid 0.01～0.03, glycyrrhizic acid 0.01～0.03, Oleum menthae 0.01～0.02, menthol 0.01～0.03, water surplus, and make that each constituent content percent sum equals 100% in the compositions.
Preparation method: by prescription, with glucide, sodium monofluorophosphate is dissolved in the water, again with Rhizoma Alpiniae Officinarum extract, and benzoic acid, glycyrrhizic acid, Oleum menthae, menthol add in the above-mentioned aqueous solution, add sodium lauryl sulfate, mix homogeneously.
Embodiment 5: slice prescription of gargling (Wt%) and preparation method
Prescription: Rhizoma Alpiniae Officinarum extract 0.5～5.0, citric acid 10.0, sodium carbonate 10.0, sodium bicarbonate 29.0, microcrystalline cellulose (A300) 10.0, sorbitol 36.0～40.5, and make that each constituent content percent sum equals 100% in the compositions.
Preparation method:,, pulverize tabletting with the above-mentioned raw materials mix homogeneously by prescription.The sheet of gargling that obtains is beautiful white, has light Rhizoma Alpiniae Officinarum fragranced.
Embodiment 6: dentifrice prescription (Wt%) and preparation method
Prescription: Rhizoma Alpiniae Officinarum extract 0.5～5.0, calcium hydrogen phosphate 56.8～61.3, calcium phosphate 35.0, sodium laurylsulfate 3.0, glucide 0.2, and make that each constituent content percent sum equals 100% in the compositions.
Preparation method: by prescription, powder fully uniform mixing in mixer earlier.Rhizoma Alpiniae Officinarum extract and glucide can be with spraying in the process of mixing and stirring behind a small amount of edible 95% dissolve with ethanol.Behind the material mixing, drying, pulverizing, mistake 80 mesh sieves can be packed.The dentifrice that obtains is beautiful white, has light Rhizoma Alpiniae Officinarum fragranced.
Embodiment 7: chewing gum formulations (Wt%) and preparation method
Prescription: gum base 40～55, Rhizoma Alpiniae Officinarum extract 0.05～5, Icing Sugar 30～40, glycerol 4～6, glucose syrup 3～6, and make that each constituent content percent sum equals 100% in the compositions.
Preparation method: by prescription, earlier gum base is moulded in moulding experienced machine put into behind the experienced elastomer-forming kneading machine knead, softening; Add glycerol, glucose, the Icing Sugar mixing of kneading successively, extrude, molding.The chewing gum that obtains has light Rhizoma Alpiniae Officinarum fragranced.
Claims (4)
1, a kind of preparation method of Rhizoma Alpiniae Officinarum extract, it is characterized in that comprising following sequential steps: it is that solvent extracts with the ethyl acetate that the Rhizoma Alpiniae Officinarum dry rhizome is pulverized the back, add ethanol in extracting solution and make aquiferous ethanol solution, in this aquiferous ethanol solution, add petroleum ether, extraction, layering, divide then and get aquiferous ethanol solution layer decolouring after-filtration, reclaim ethanol and be concentrated into driedly, obtain counting by weight percentage and contain galangin 1～25%, the Rhizoma Alpiniae Officinarum extract of total flavones＞10%.
2, Rhizoma Alpiniae Officinarum extract preparation method according to claim 1 is characterized in that: percentage calculation by volume in the described aquiferous ethanol solution, ethanol content is 70～75%.
3, Rhizoma Alpiniae Officinarum extract preparation method according to claim 1 is characterized in that: described petroleum ether is the petroleum ether of 60～90 ℃ of boiling ranges.
4, Rhizoma Alpiniae Officinarum extract preparation method according to claim 1 is characterized in that: in the described decolouring step, be incorporated as 0.5～5% active carbon with mass fraction calculating in the aquiferous ethanol solution layer.
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| CN103735466B (en) * | 2014-01-15 | 2015-10-28 | 中国热带农业科学院农产品加工研究所 | A kind of galangal hydrolat healthcare collutory and preparation method thereof |
| CN105054066B (en) * | 2015-08-19 | 2018-05-01 | 中国热带农业科学院农产品加工研究所 | A kind of galangal rhizome extract and its preparation method and application |
| CN105166308A (en) * | 2015-08-27 | 2015-12-23 | 济南舜祥医药科技有限公司 | Ginger-flavored chewing gum and preparation method thereof |
| CN107308081A (en) * | 2017-07-11 | 2017-11-03 | 景雷 | A kind of strong bactericidal mouthwash |
| CN108635310B (en) * | 2018-08-14 | 2021-04-20 | 海南金香远药业科技有限公司 | Anti-inflammation toothpaste and preparation method thereof |
| CN116195619A (en) * | 2023-02-28 | 2023-06-02 | 珠海市自然之旅生物技术有限公司 | Spore inhibition compound composition and preparation method and application thereof |
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| 天然化学成分高良姜素研究进展. 何瑞等.时珍国医国药，第10卷第10期. 1999 |
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