CN100548970C - The extraction process of total amino acid and other salt-base substances in the garlic - Google Patents
The extraction process of total amino acid and other salt-base substances in the garlic Download PDFInfo
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- CN100548970C CN100548970C CNB2004100681536A CN200410068153A CN100548970C CN 100548970 C CN100548970 C CN 100548970C CN B2004100681536 A CNB2004100681536 A CN B2004100681536A CN 200410068153 A CN200410068153 A CN 200410068153A CN 100548970 C CN100548970 C CN 100548970C
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Abstract
The present invention relates to extract the efficient part of preparation garlic, comprise that promptly multiple garlic contains methyllanthionine and their dipeptide, its preparation process comprises the various enzymes of (1) inactivation, (2) degreasing, (3) extracting, (4) precipitation or ultrafiltration, (5) ion-exchange enrichment, (6) decolouring, (7) each step of re-refining.The product of this explained hereafter, yield 2-4%, total amino acid content are more than 80%, more than the alliin content 5-10%, to be used to make the oral and injection of medicine of health products.
Description
Technical field
The present invention relates to a kind of preparation method who from garlic, extracts total position of total amino acid (comprising a large amount of sulfur-containing amino acid and general amino acid) and other salt-base substances.
Background technology
Garlic is a liliaceous plant, formal name used at school Allium salivum, its phosphorus stem is China people medicine-food two-purpose since ancient times, modern medicine proof garlic has antithrombotic, suppress platelet aggregation, it is synthetic to suppress cholesterol in human body, the anti-inflammatory bacterium, effect (the WHO monographs on selectedmedicinal plants vol.1 of antiviral and chemoprevention of cancer, P.16-32, World Health Organization, Geneva) all closely related with sulfocompound wherein (A.Kamel and M.Saleh:Studies in Natural Products Chem.Vol 23.P 455-485.Atta-ur-Rahman edits 2000, Elsevier) for (the Commission E monographsP.134 July of the Bundesgesundheitsamt Deutschland.E council of Germany board of health 06.1988) and these health care and therapeutic action.
Sulfocompound in the garlic comprises halfcystine and derivative (methyl halfcystine thereof, the S-1-allyl cysteine, the S-2-allyl cysteine, propylcysteine, methionine(Met) and their oxidized form sulfoxide compound Sulfoxide) and the dipeptide formed of these amino acid; The enzyme that these sulfur-containing amino acid and peptide exist in garlic (comprises various peptidohydrolases, peptide saccharase, gamma-glutamic acid peptide saccharase particularly, the hydrogen peroxide oxidation enzyme, allinase etc.) can change into allicin Allicim under the effect, because allicin unstable chemcial property, can further react again and generate Ajoene class, dithiine class, polytype compounds such as thioether class.
The early stage both at home and abroad exploitation of garlic mainly being concentrated provides the sulfur-bearing volatile oil, i.e. allicin and further reaction product.Then more pay attention to wherein high-load sulfur-containing amino acid closely during the last ten years.Such as the exploitation of the primary medicinal powder of garlic, particularly use lyophilize production, with the oral preparations of the deodorised garlic powder that keeps the high-content sulfur-containing amino acid with as healthcare products and medicine.
Because above-mentioned sulfur-containing amino acid is that multiple compound of the same type exists jointly, and their unstable chemically.Make the drug effect worker be difficult to obtain the high purity sample and carry out bioassay.Therefore above-mentioned these drug effects are studied carefully which kind of compound generation of genus, their pharmacology is tired, structure activity relationship, mutual synergy ... etc. problem, much still imperfectly understand at present, add that current international and domestic understanding major part to plant amedica (Chinese medicine) curative effect tends to think the coefficient result of various chemical components.
Summary of the invention
The object of the present invention is to provide a kind of method that wherein total sulfur-containing amino acid comprises the mixing position of general amino acid and salt-base substances of from garlic, extracting.
The present invention comprises that for providing systems technology to be used to produce the position of garlic total amino acid and other alkali sexual element is used to produce various oral healthcare products and therapeutical agent, and can be again through refining production injection or the intravenous drip usefulness of being used for.
The used garlic raw material of this technology can be fresh garlic, dried garlic slice, and yield can be because of the place of production of crude drug raw material and Mining storage condition different between the time receiving, and general fresh garlic production yield is 2-4%, and dried garlic slice production yield is 3-5%.
Technology of preparing provided by the invention comprises the following steps:
1, inhibitory enzyme activity
(a)) the fresh garlic raw material made various enzyme deactivations in 30 minutes in 150 ℃ of bakings.
(b) the fresh garlic raw material immerses in the boiling water or the water proof boiling, keeps boiling 30 minutes to 45 minutes, to guarantee various enzyme complete deactivations.
2, degreasing
Garlic behind inhibitory enzyme activity adds suitable quantity of water and blends, and with the chloroform degreasing, with weeding of grease soluble substance part, the degreasing of this technology can be used haloalkane, C
1-C
5Lower member ester, C
1-C
5Organic solvents such as rudimentary ether: as sherwood oil, chloroform, tetracol phenixin, methylene dichloride, ethylene dichloride, ethyl acetate, butylacetate, methylethylketone, ether, benzene or toluene etc.
3, extract
The extraction agent of the garlic juice after degreasing is a water, or moisture water-soluble solvent such as aqueous methanol, aqueous ethanol, moisture propyl alcohol adds the about 10-20 of solvent and doubly measure, and warm lixiviate was got 2 hours, filter, filter residue repeats to extract once, and united extraction liquid extracts and can be 50-90% with determining alcohol.
4, solvent deposition and film are handled:
Through water or hydrous alcohol extraction gained solution membrane ultrafiltration, collect filtered solution (film of 3,000-50,000 molecular weight can be the boundling hollow-fibre membrane, flat sheet membrane, rolled film and ceramic membrane etc.) and remove the polymer substance of holding back with 3,000-50,000 molecular weight.
5, ion-exchange: above-mentioned treatment solution is by polystyrene type macropore sulfonic acid ion exchange resin, for example strong positive ion exchange resin such as D001, HD-82, D061, S-9 make amino acid, the sorption of biogenic amine isoreactivity material on resin, water or 50% alcohol are washed post again, the flush away carbohydrate, the soap class, the neutrality of non-amino acids such as aldehydes matter or acidic substance, the resin column of cleaning is with 1-5% ammoniacal liquor or ammonia ethanol elution, present alkalescence to elutriant, negative until the triketohydrindene hydrate qualitative reaction, be evaporated to 1/3 volume, remove excess of ammonia water.
6, charcoal absorption
Add proper amount of active carbon further to remove the pigment material, filter, filtrate is washed with water or 50% ethanol again, is evaporated to the small volume spraying drying, is this efficient part, is micro-yellow powder.
7, refining
As injection or intravenous drip usefulness, should further make with extra care, and remove wherein thermal source and protein, method is for repeating the primary ions exchange and handle and again through a membrane filtration, concrete grammar being the same.
The Chemical Composition that comprises in the product has:
(1) sulfur-containing amino acid: halfcystine Cysteine, methyl halfcystine S-methyl cysteine (SMC), sulphur-1-allyl cysteine S-1-propenyl cysteine, sulphur-2-allyl cysteine, S-2-propenyl cysteine (being that S-allyl cysteine S-allyl cysteine is called for short SAC), thiopropyl hemiamic acid S-propanyl cysteine, methionine(Met) Metheonine and their sulfoxide class, such as sulphur-2-allyl cysteine sulfoxide (alliin Alliin), sulphur-1-allyl cysteine sulfoxide (being different alliin isoalliin) methionine sulfoxide Methiin cycloalliin cycloalliin etc.
(2) common amino acid: the dipeptides that glycine, L-glutamic acid, leucine, Isoleucine, proline(Pro), phenylalanine, arginine, Aspartic Acid, Methionin, 2,5-diaminovaleric acid, Serine, methionine(Met) and above-mentioned these amino acid (particularly L-glutamic acid and above-mentioned sulfur-containing amino acid) constitute, the relative content of above-mentioned sulfur-containing amino acid and peptide can be because of the different places of production of garlic raw material, acquisition time, the difference of storage condition and time and different (seeing Table 1).
Qualitative making known and also contained a spot of allicin and degraded product thereof in this position in addition, the selenoamino acid and the degraded product thereof of trace, alkamines compound.
This product is faint yellow solid, and is soluble in water, methyl alcohol and aqueous ethanol, be insoluble in trichloromethane, tetracol phenixin, methylene dichloride, ethyl acetate, butylacetate, methylethylketone, ether is pressed the analytical data that this product is numbered Ex-A 040224 product in the organic solvents such as sherwood oil.
The amino acid analysis report
Free 22.93mg/10ml
Measure common amino acid content with automatic analyzer for amino acids
Free aminoacid content 36.30% hydrolysising amino acid content 76.35%
Alliin content with reference to American Pharmacopeia USP25 version (2004) Official Monographys P.2550Garlic down the method for Content of alliin regulation to measure control sample be 8.6% for synthetic alliin according to a conventional method through purifying mensuration alliin content repeatedly.
Can produce medicine with fresh garlic or dried garlic slice with this explained hereafter healthcare products, requirement selects for use the garlic raw material of the specific place of production and storage practice clear, constant and controlled to guarantee 50% above Chemical Composition, be used to produce injection and remove the high-quality garlic raw material of selecting the specific place of production and storage practice for use, and need the oral preparations raw material is further purified, particularly the membrane filtration purifying is to reach 80% above Chemical Composition, clear, constant, controlled, remove wherein pyrogen and protein, and meet the finger printing code requirement of national regulation.
Description of drawings
Fig. 1 is the product amino acid finger printing that extracts.
Fig. 2 is the HPLC figure of alliin.
Embodiment
Below in conjunction with embodiment the present invention is further described, but does not limit the present invention.
Embodiment (one)
Remove the peel 500 gram garlic bulb lobes then, put into and boiled in 2500 ml waters 30 minutes, kill the garlic biological enzyme, keep the complete of garlic during this period.Kill and from water, pull out after enzyme is finished, naturally cool to room temperature.Stirred simultaneously ten minutes killing the garlic bulblet pulverizing of enzyme and the trichloromethane or the methylene dichloride of adding qdx, after finishing, slag, liquid are separated, and liquid portion divides water-yielding stratum with liquid liquid separator, garlic tissue and water layer partly again with trichloromethane or ethylene dichloride degreasing once.The garlic of degreasing and water are added into 15 times of water, heating lixiviate 2 hours, and temperature is controlled between 40～70 degree, after extraction finishes, with suction method slag liquid is separated, and collects vat liquor.Slag adds 15 times of above again method lixiviates of water gaging once again, and slag liquid separates, and merges vat liquor twice.Vat liquor is earlier with the particulate in the 0.1 micron membranes elimination vat liquor, and then with 3,000 or 5,000 molecular weight ultra-filtration membrane ultrafiltration, the ultrafiltration temperature be controlled at 25 spend about, pressure-controlling is at 2～3kg.Liquid is passed through in collection.By the liquid concentrating under reduced pressure, thickening temperature is controlled at 50 degree, emits when being concentrated to 2000 ml volumes and naturally cools to room temperature.
Above-mentioned concentrated solution is by D001 ion exchange resin, and resin demand is 500 milliliters, and resin will clean and be processed into Hydrogen before being used.Feed liquid is passed through with the flow velocity of about 30 milliliters of per minutes.After having led to feed liquid, resin is with the washed with de-ionized water raffinate of two bed volumes, uses the 50% ethanol flush away of two bed volumes may be by the carbohydrate of resin absorption again, glucosides class material.With 1% ammoniacal liquor wash-out, be negative as qualitative reaction with triketohydrindene hydrate subsequently until elutriant.Elutriant merges concentrating under reduced pressure, is concentrated into and removes ammoniacal liquor unnecessary in the solution about 250 milliliters.Concentrated solution adds an amount of granulated active carbon, stirs 30 minutes, and is static more than 3 hours, and with 0.45 micrometer nylon membrane filtration, filtrate decompression is concentrated into dried, gets little yellow garlic efficient part 20.3 grams.Through content analysis, wherein alliin content is 8.6%.Aminoacids content is greater than 80%.
Embodiment (two):
Next year peeling garlic bulb lobe 500 restrains, and biological enzyme was killed in the water proof boiling in 30 minutes, kills to naturally cool to room temperature after enzyme is finished.The garlic bulblet that killed enzyme pulverized and add the methylethylketone of qdx or ethyl acetate soaking and stirring 10 minutes, the static degreasing of spending the night.Second angel's slag liquid separates, and liquid portion divides with liquid liquid separator and removes methylethylketone or ethyl acetate, garlic tissue and water liquid partly again with methylethylketone or ethyl acetate degreasing once.Garlic after the degreasing adds 15 times of 50% methanol eddy extracts 2 times, and each 2 hours, after extraction finishes, melt cinder is separated, collect extracting solution.Merge extracted twice liquid concentrating under reduced pressure, be concentrated into and contain the alcohol amount less than 10%.Concentrated solution is used 10,000 or 30,000 molecular weight ultra-filtration membrane ultrafiltration more earlier with the particulate in the 0.1 micron membranes elimination extracting solution, and the ultrafiltration temperature is controlled at 25 degree, and pressure-controlling is about 2kg.Liquid is passed through in collection.Merge concentrating under reduced pressure by liquid, thickening temperature is controlled at 50 degree, emits when being concentrated to 2000 milliliters and naturally cools to room temperature.
Above-mentioned concentrated solution is by HD-82 ion exchange resin, and resin demand is 500 milliliters, and feed liquid is passed through with the flow velocity of about 30 milliliters of per minutes.After feed liquid was passed through, resin was with the deionized water flush away raffinate of two bed volumes, used the 50% ethanol flush away of two bed volumes may be by the carbohydrate of resin absorption again, glucosides class material.Subsequently with 5% ammonia ethanol elution; be negative as qualitative reaction with triketohydrindene hydrate until elutriant; elutriant merges concentrating under reduced pressure, is concentrated into about 250 milliliters, remove ammoniacal liquor unnecessary in the solution after; the an amount of granulated active carbon that adds in concentrated solution; stirred 30 minutes, static more than 3 hours, with 0.45 micrometer nylon membrane filtration; filtrate decompression is concentrated into dried, gets little yellow garlic efficient part 11.7 grams.Through content analysis, wherein alliin content is 5.1%, and aminoacids content is greater than 80%.
Embodiment (three):
Peeling garlic bulb lobe 500 restrains then, place 150 degree baking boxs to kill enzyme in interior 30 minutes, to be cooled to room temperature, put in qdx ethylene dichloride or the tetracol phenixin, pulverizing and boiling reflux 30 minutes, degreasing, ethylene dichloride or tetracol phenixin are removed with vacuum filtration in the back of refluxing, divide water-yielding stratum with liquid liquid separator, with method operation secondary.Garlic after the degreasing and the water layer of telling are added 15 times of 30% propyl alcohol, and hot dipping is carried 4 hours, and temperature is about 60 degree, and after extraction finished, extracting solution was collected in centrifugal slag liquid separation.Newly add 15 times of 30% above again method extracting of propyl alcohol in the slag once, slag liquid separates.Merge extracted twice liquid concentrating under reduced pressure, temperature is controlled at about 50 degree, is concentrated to contain the alcohol amount and end less than 10%, leaves standstill cool to room temperature.Then with the particulate in the 0.1 micron membranes elimination concentrated solution, and then with 50,000 molecular weight ultra-filtration membrane ultrafiltration, the ultrafiltration temperature is controlled at 25 and spends, and pressure-controlling is at 2～3kg.Liquid is passed through in collection.By the liquid concentrating under reduced pressure, thickening temperature is controlled at 50 degree, emits when being concentrated to 400 ml volumes and naturally cools to room temperature.
Above-mentioned concentrated solution is the D061 Zeo-karb by the strongly acidic styrene, and resin demand is 500 milliliters, and resin is treated to Hydrogen before feeding feed liquid, and feed liquid is passed through with the flow velocity of about 30 milliliters of per minutes.After feed liquid was passed through, resin was with the deionized water flush away raffinate of two bed volumes, used the 50% ethanol flush away of two bed volumes may be by the carbohydrate of resin absorption again, glucosides class material.With 5% ammoniacal liquor wash-out, be negative as qualitative reaction with triketohydrindene hydrate until elutriant subsequently, elutriant merges concentrating under reduced pressure, is concentrated into about 1 liter to remove ammoniacal liquor unnecessary in the solution.Concentrated solution adds an amount of granulated active carbon, stirs 30 minutes, and is static more than 3 hours, and with 0.45 micrometer nylon membrane filtration, filtrate decompression is concentrated into dried, gets little yellow garlic efficient part 13.1 grams.Through efficient liquid phase chromatographic analysis, wherein alliin content is 5.7%, and total amino acid content is greater than 80%.
Embodiment (four):
Garlic bulb dry plate 1000 gram adds 20 times of amount 50% ethanol and pulverizes and refluxed two hours, extracts, and refluxes and finishes, and centrifugation melt cinder, slag add 15 times of amount 50% ethanol and reflux once again, and slag liquid separates.Extracting solution vacuum concentration, temperature are controlled at 50 degree, are concentrated to about 4 liters to contain alcohol hardly at this moment, naturally cool to room temperature.Cooling fluid is with organic solvent extraction secondaries such as each 500 milliliters of butylacetates or ether, degreasing.The further concentrating under reduced pressure of water liquid that took off fat adds 2000 milliliter of 95% ethanol or Virahol, alcohol precipitation while hot to small volume in the time of about 1000 milliliters, placement is spent the night, and gets light liquid, concentrating under reduced pressure, thickening temperature is controlled at 50 degree, emits when being concentrated to 1000 milliliters and naturally cools to room temperature.
Above-mentioned concentrated solution is by S-9 ion exchange resin, and resin demand is 1000 milliliters, and resin is treated to Hydrogen before feeding feed liquid, and feed liquid is passed through with the flow velocity of about 30 milliliters of per minutes.After feed liquid was passed through, resin was with the deionized water flush away raffinate of two bed volumes, used the 50% ethanol flush away of two bed volumes may be by the carbohydrate of resin absorption again, glucosides class material.With 3% ammoniacal liquor wash-out, be negative as qualitative reaction with triketohydrindene hydrate until elutriant subsequently, elutriant merges concentrating under reduced pressure, is concentrated into about 1 liter to remove ammoniacal liquor unnecessary in the solution.It is an amount of to add granulated active carbon in the concentrated solution, stirs 30 minutes, and static more than 3 hours, with 0.45 micrometer nylon membrane filtration, filtrate decompression is concentrated into dried, gets little Huang or light brown garlic efficient part 51.6 grams.Through efficient liquid phase chromatographic analysis, wherein alliin content is 6.2%, and total amino acid content is greater than 80%.
Claims (7)
1, a kind of extraction process of extracting the preparation total amino acid from garlic comprises a, inhibitory enzyme activity; B, degreasing; C, extraction; D, solvent deposition and film are handled; E, ion-exchange; F, charcoal absorption; G, refining.
2, extraction process according to claim 1 is characterized in that using baking, scalds and boil or the operation of boiling makes all kinds of biological enzyme inactivation in the garlic.
3, extraction process according to claim 1 is characterized in that degreasing employing halogenated alkane, methylethylketone, ethyl acetate, ether, benzene or toluene.
4, extraction process according to claim 1, the extraction agent that it is characterized in that extracting the garlic total amino acid are water or aqueous methanol, aqueous ethanol, moisture propyl alcohol.
5, extraction process according to claim 1 is characterized in that film handle to adopt the ultra-filtration membrane of 3,000 molecular weight to five, ten thousand molecular weight.
6, extraction process according to claim 1, the strong cationic resin that it is characterized in that being used for ion-exchange is a polystyrene type macropore sulfonic acid ion exchange resin.
7, extraction process according to claim 6 is characterized in that polystyrene type macropore sulfonic acid ion exchange resin is D001, HD-82, D061 or S-9 strong positive ion exchange resin.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150004658A1 (en) * | 2012-03-14 | 2015-01-01 | Nisshin Pharma Inc. | Sulfur amino acid-containing composition |
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| CN103159844B (en) * | 2011-12-19 | 2015-01-07 | 中国科学院生物物理研究所 | Method capable of reducing immunotoxicity of venom nerve growth factor and enabling immunotoxicity to be drug alternative of mouse origin nerve growth factor |
| CN105541681B (en) * | 2015-12-24 | 2017-09-29 | 青岛自然珍萃生物科技有限公司 | A kind of preparation method of high content alliin |
| CN111529467B (en) * | 2020-05-30 | 2020-12-22 | 欧露莲生物科技(广东)有限公司 | A garlic extract containing protein peptide for cosmetic and its preparation method |
| CN112760350A (en) * | 2021-02-06 | 2021-05-07 | 巨野恒丰果蔬有限公司 | Preparation method of garlic antihypertensive peptide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20150004658A1 (en) * | 2012-03-14 | 2015-01-01 | Nisshin Pharma Inc. | Sulfur amino acid-containing composition |
| US9340808B2 (en) * | 2012-03-14 | 2016-05-17 | Nisshin Pharma Inc. | Sulfur amino acid-containing composition |
| TWI585206B (en) * | 2012-03-14 | 2017-06-01 | Nisshin Pharma Inc | A method for producing a composition containing a sulfur-containing amino acid |
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