CN101745008B - Extraction method of ginseng, ophiopogon root and shiandra and preparation thereof - Google Patents
Extraction method of ginseng, ophiopogon root and shiandra and preparation thereof Download PDFInfo
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- CN101745008B CN101745008B CN 200810153789 CN200810153789A CN101745008B CN 101745008 B CN101745008 B CN 101745008B CN 200810153789 CN200810153789 CN 200810153789 CN 200810153789 A CN200810153789 A CN 200810153789A CN 101745008 B CN101745008 B CN 101745008B
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Abstract
The invention relates to a Chinese traditional medicine extraction method and a pharmaceutical preparation thereof, in particular to a preparation for treating cardiovascular diseases, tonifying qi and calming pulse and a preparation method thereof. The preparation is prepared from ginseng, ophiopogon root and shiandra.
Description
Technical field:
The present invention relates to a kind of Traditional Chinese medicine extraction method and pharmaceutical preparation thereof, particularly qi-tonifying and pulse-restoring preparation of a kind of Cardiovarscular and preparation method thereof, said preparation are by Radix Ginseng, and Radix Ophiopogonis and Fructus Schisandrae Chinensis three flavor Chinese drug preparations form.
Background technology:
Radix Ginseng is the root of Araliaceae Radix Ginseng Panax ginseng C.A.Mey..Sweet, the little hardship of its property of medicine, flat, return lung, spleen, heart channel; Its effect strongly invigorating primordial QI, invigorating the spleen to benefit the lung promotes the production of body fluid, the Fructus Alpiniae Oxyphyllae of calming the nerves.Use: the vigour collapse has been demonstrate,proved, lung spleen heart syndrome of deficiency of kidney-QI, and calentura deficiency of vital energy Tianjin wound reaches diabete yearningly.Its chemical constituent comprises multiple ginsenoside, volatile oil, aminoacid, trace element and organic acid, saccharide, vitamin etc.
Have another name called dwarf lilyturf, book band grass Radix Ophiopogonis, be Liliaceae Ophiopogon perennial evergreen herbaceous plant.Fibrous root is more sturdy, and often expand at the top of root or middle part becomes spindle shape meat fritter.Its nature and flavor with return through: sweet, little hardship is slightly cold GUIXIN, lung, stomach warp.Its function with cure mainly: YIN nourishing and the production of body fluid promoting, lung moistening clears away heart-fire, and is used for dryness of the lung dry cough, the chronic consumptive disease cough, Tianjin wound is thirsty, vexed insomnia, interior-heat is quenched one's thirst, dryness of the intestine constipation, pharyngeal diphtheria.Its chemical constituent comprises Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins etc.
Fructus Schisandrae Chinensis is commonly called as Fructus Zanthoxyli Plansipini, sliding weight of steelyard, medicine Fructus Schisandrae Chinensis, face rattan, five Fructus Armeniacae Mumes etc., ancient medical book Cheng Ta Chi Zhu, profound and, can and.It is the fruit of magnoliaceae schisandra.Schisandra fruit implementation Chinese medicine function supplementing QI for promoting the production of body fluid, the nourishing kidney of astringing the lung, antidiarrheal, arresting seminal emission, calm the nerves, can control the diseases such as chronic cough dyspnea due to deficiency, the few xerostomia in Tianjin, seminal emission chronic diarrhea, forgetful insomnia.The pharmacological testing proof can be regulated central nervous system's excitement and process of inhibition, promotes body metabolism, regulates the secretion of gastric juice and bile, and hepatitis convalescent period transaminase rising person is had reducing effect.Peel and the ripe skin of planting contain lignanoid, are the effective medicinal components of Fructus Schisandrae Chinensis, comprising multiple schizandrin.Seed is fatty, but oils and fats soap system or machine oil.Stem and leaf and seed all can extract aromatic oil.
Qi-tonifying and pulse-restoring preparation derives from the ancient prescription SHENGMAI SAN, SHENGMAI SAN source " medicine origin ", it is by Radix Ginseng, Radix Ophiopogonis, Fructus Schisandrae Chinensis forms, have supplementing QI and nourishing YIN, multiple arteries and veins takes off admittedly, clinically is usually used in treating that acute myocardial infarction, cardiogenic shock, toxic shock, hemorrhagic shock and coronary heart disease, endocrine disturbance etc. are sick belongs to the deficiency of both QI and YIN persons.
Existing qi-tonifying and pulse-restoring preparation extraction process is as follows:
Chinese patent CN200310116732.9 discloses a kind of method for preparing the Shengmai for injection lyophilized injectable powder, first to Fructus Schisandrae Chinensis 60-80% alcohol reflux 2-3 time, each 60-120min, Recycled ethanol is to thing alcohol flavor, extractum under agitation adds ethanol, make the alcohol amount of containing reach 60-80%, filter, concentrating under reduced pressure gets extracting solution A; Again with Fructus Schisandrae Chinensis medicinal residues and Radix Ginseng behind the ethanol extraction, adding hydration Radix Ophiopogonis fries in shallow oil, after the merging aqueous extract is concentrated, again through precipitate with ethanol, filter, after doubly measuring deionized water dissolving with 10-15 behind the Recycled ethanol, process with macroporous adsorbent resin, be washed till sugar-free with deionized water first, be washed till without Saponin with ethanol again and end, reclaim alcohol eluen, concentrate to get extracting solution B; With above-mentioned Radix Ginseng, the precipitation adding distil water dissolving behind Radix Ophiopogonis and the Fructus Schisandrae Chinensis water extract-alcohol precipitation filters, and drying gets the water extraction polysaccharide crude, with the dissolving of polysaccharide crude adding distil water, crosses hollow fiber column ultrafilter, gets extracting solution C.
Chinese patent CN200410057331.5 discloses a kind of method for preparing Shengmai injection, Radix Ginseng ethanol extraction three times, merge extractive liquid,, concentrating under reduced pressure, add water to medical material than 1: 1, separate and remove upper strata oil, filter, concentrated, vacuum drying gets Radix Ginseng extract; Radix Ophiopogonis and Fructus Schisandrae Chinensis decoct with water respectively, merge extractive liquid,, and concentrating under reduced pressure adds ethanol, places, and filters, filtrate decompression is concentrated, adds ethanol again, places, and filters, and regulates pH value, places, filter, adjust pH again, reclaim under reduced pressure, vacuum drying, respectively Radix Ophiopogonis, Fructus Schisandrae Chinensis extrat.
Chinese patent CN200410021920.8 discloses a kind of preparation method of qi-tonifying and pulse-restoring preparation, the Radix Ginseng Rubra ethanol extraction, and Recycled ethanol, aqueous precipitation filters, and concentrated, vacuum drying, spray drying or lyophilization get Radix Ginseng Rubra extract; Radix Ophiopogonis, Fructus Schisandrae Chinensis water extraction, after extracting solution is concentrated, precipitate with ethanol, Recycled ethanol, medicinal liquid is concentrated, use again vacuum drying, spray drying or freeze-drying dry, get Radix Ophiopogonis, Fructus Schisandrae Chinensis extrat.
Chinese patent CN96117457.9 discloses a kind of SHENGMAI ZHUSHEYE and preparation method thereof, gets Radix Ginseng Rubra and mixes with Radix Ophiopogonis, uses alcohol dipping, filters, and alcohol reflux extracts; Fructus Schisandrae Chinensis with vapor distillation, decocting boil, alcohol precipitation extracts.
Chinese patent CN200310121126.6 discloses a kind of Shengmai for injection and preparation method thereof, and the source method is oozed in the medicinal component employing of Radix Ginseng Rubra, alcohol reflux boils the extraction that combines with decocting; The medicinal component of Radix Ophiopogonis adopts alcohol reflux to boil the extraction that combines with decocting; The medicinal component of Fructus Schisandrae Chinensis adopts water distillation, alcohol reflux to boil the extraction that combines with decocting; The extraction process flow process is as follows: (1) Radix Ginseng Rubra adopts first ethanol to ooze the source and extracts, and gets Radix Ginseng Rubra extracts active ingredients liquid a; To ooze subsequently the Radix Ginseng Rubra that extracted in the source and use again alcohol reflux, get Radix Ginseng Rubra extracts active ingredients liquid b; The Radix Ginseng Rubra water boiling and extraction of again alcohol reflux being crossed filters, and then precipitate with ethanol after filtrate is concentrated is got supernatant and filtered, filtrate and above-mentioned a, b merge, and cold preservation is got supernatant and filtered, then water precipitating after filtrate is concentrated is got supernatant and is filtered, and namely gets the medicinal component extracting solution of Radix Ginseng Rubra C; (2) adopt first alcohol reflux Radix Ophiopogonis, cold preservation is got supernatant and is filtered, and water precipitating after filtrate is concentrated is got supernatant again and filtered, and namely gets extracts active ingredients liquid d Radix Ophiopogonis; Use water boiling and extraction the Radix Ophiopogonis that again alcohol reflux is crossed, filter, precipitate with ethanol after filtrate is concentrated, then get supernatant and filter, Recycled ethanol also is concentrated into thick paste shape, water precipitating, then getting supernatant filters, namely get medicinal component extracting solution e Radix Ophiopogonis: with extracts active ingredients liquid d and e merging Radix Ophiopogonis, filter, namely get medicinal component extracting solution f Radix Ophiopogonis; (3) the Fructus Schisandrae Chinensis distillate adopts the Fructus Schisandrae Chinensis steam distillation, collect distillate and namely get Fructus Schisandrae Chinensis distillate g: the Fructus Schisandrae Chinensis behind the collection distillate adopts first alcohol reflux, cold preservation, getting supernatant filters, filter concentrated rear water precipitating, getting supernatant filters, namely get Fructus Schisandrae Chinensis extracts active ingredients liquid h: the Fructus Schisandrae Chinensis water boiling and extraction of again alcohol reflux being crossed, filter, then secondary precipitate with ethanol after filtrate is concentrated is got supernatant and is filtered, Recycled ethanol also is concentrated into the thick paste shape, then water precipitating goes supernatant to filter, and namely gets the medicinal component extracting solution of Fructus Schisandrae Chinensis i; Fructus Schisandrae Chinensis extracts active ingredients liquid g, h and i are merged, filter, namely get the medicinal composition extracting solution of Fructus Schisandrae Chinensis j.
Chinese patent CN99114091.5 discloses medicine of a kind of cardiovascular diseases for the treatment of and preparation method thereof, Radix Ginseng, Radix Ophiopogonis, Fructus Schisandrae Chinensis is added hydration fry in shallow oil; Aqueous extract or eluent are through ethanol or acetone precipitation; Macroporous resin treatment; Ion exchange resin treatment; Separate the effective ingredient that obtains extract.
Chinese patent CN200510088087.3 discloses a kind of Activating Pulse Injecting Preparation And Preparation Method, the preparation method of Radix Ginseng Rubra extract adopts conventional ethanol refluxing process to extract, the preparation method of Fructus Schisandrae Chinensis extrat is, get the water extraction 3 times that schisandra chinensis medicinal material adds 6 times of amounts, each 40min filters, merging filtrate, be concentrated into relative density 1.10～1.15, add 95% ethanol and carry out ethanol precipitation twice, make for the first time to contain the alcohol amount and reach 80%, make for the second time and contain the alcohol amount and reach 85%, filter, merging filtrate, decompression recycling ethanol is to relative density 1.10～1.15, adding water stirs evenly, leave standstill, filter, filtrate adding w/v is 0.4% active carbon, boil, keep little 30nin that boils, slightly cold filtration, this technique is not extracted the volatile oil composition in the schisandra chinensis medicinal material; The preparation method of Radix Ophiopogonis extract is: get medical material Radix Ophiopogonis, filter behind the water boiling and precipitation with ethanol, add water behind the filtrate recycling ethanol and stir evenly, leave standstill, filter, get filtrate A, the precipitation of precipitate with ethanol is dissolved in water, leave standstill, filter, get liquor B, filtrate A and B are merged, add charcoal treatment, filter, this technique has been extracted the polysaccharide composition in medical material Radix Ophiopogonis.Chinese patent CN2005100081662.7 discloses a kind of Activating Pulse Injecting Preparation And Preparation Method, with Radix Ginseng Rubra medical material section, measures 60%～90% alcohol reflux 1～5 time with 5～10 times, each 0.5～3 hour, merge backflow, filter, decompression filtrate recycling ethanol to relative density is 1.10～1.15, the gained thick paste adds water, stirs evenly, and 2～SOC left standstill 6～20 hours, filter, filtrate is used charcoal treatment, filters, and gets filtrate A for dosing; Get each medical material of wheat, add 5～10 and borrow the water extraction 1～4 time of amount, each 20～90min, filter, it is 1.05～1.10 that filtrate is concentrated into relative density, adds 95% ethanol and carries out ethanol precipitation twice, make for the first time to contain the alcohol amount and reach 80%, make for the second time to contain the alcohol amount and reach 85%, filter, decompression filtrate recycling ethanol to relative density is 1.10～1.15, adds water, stirs evenly, put 6～20 hours, filter, get liquor B 1, with the precipitation merging of ethanol precipitation twice, add the water for injection dissolving, left standstill 6～20 hours, and filtered, get liquor B 2, liquor B 1 and B2 are merged, adding w/v is the charcoal treatment of 0.1-3%, filters, and gets liquor B for dosing; Schisandra chinensis medicinal material adds the water extraction 1～4 time of 4～8 times of amounts, and each 20～90min filters, merging filtrate, being concentrated into relative density is 1.10～1.15, the gained thick paste adds 95% ethanol and carries out ethanol precipitation twice, make for the first time to contain the alcohol amount and reach 80%, make for the second time to contain the alcohol amount and reach 85%, filter, merging filtrate, decompression recycling ethanol to relative density is 1.10～1.15, adds water, stir evenly, leave standstill, filter, filtrate with charcoal treatment after, filter, get liquor C for dosing; With filtrate A, B, C mixing, make different preparations according to conventional method.
Complex manufacturing in the prior art, cost is high, and the problem that extraction ratio is low never is overcome.
The present invention has overcome the shortcoming of existing extraction process through for a long time research, and it is high to have invented a kind of effective component extraction rate, good stability, and dosage is few, instant effect, cost is low, is easy to the long-time extracting method of preserving.
Summary of the invention:
The invention provides a kind of new Yiqi and vein recovery extract and preparation method thereof.
The Yiqi and vein recovery prescription is: 1 part of Radix Ginseng, 3 parts of Radix Ophiopogonis, 1.5 parts of Fructus Schisandrae Chinensis, described part is weight portion.
Wherein Radix Ginseng is Radix Ginseng Rubra or Radix Ginseng, preferred Radix Ginseng Rubra.Fructus Schisandrae Chinensis is Radix Schisandrae Bicoloris or Fructus Schisandrae Sphenantherae, preferred Radix Schisandrae Bicoloris.
Preparation method of the present invention comprises 1 part of Radix Ginseng, 3 parts of Radix Ophiopogonis, 1.5 parts of Fructus Schisandrae Chinensis, first three flavor Chinese medicines is extracted separately, mixes singly carrying thing afterwards.
Described singly carry refer to three flavor Chinese medicines respectively water extract or extract separately with alcohol extraction.
Wherein refer to be soaked in water with water extraction or water heating is boiled and carried or the water heating and refluxing extraction,
Refer to use the solvent that contains ethanol or other alcohols materials to use with alcohol extraction and soak, percolation, the modes such as reflux are extracted, and wherein preferred alcohol is ethanol, and ethanol can be the ethanol of 30%-100% concentration.
Preparation method of the present invention also comprises the further water of medicinal residues after extracting for the first time or for the second time or the step of alcohol extraction.
Preparation method of the present invention also comprises the extraction product after extracting is separated step with purification.
Described separation and purification comprise precipitation, filter washing, chromatography, the methods such as recrystallization.
For this reason, preparation method of the present invention preferably adopts following methods
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule or coarse powder are cut into slices, are ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 6-10 and doubly measure aquiferous ethanol, preferred 6 times of amounts, the preferred 10-70% of aquiferous ethanol concentration, preferred 40%;
(3) boil extraction 1-5 time, each 1-3 hour, extracting solution merged;
(4) better, can decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, adds ethanol, and making determining alcohol is 50-80% (preferred 70%), can cold preservation 8～15 hours (preferred 12 hours), filter, and concentrated, get extractum, obtaining product is that the Radix Ginseng list is carried thing;
Wherein step 5 also can be with concentrating to get extractum behind the n-butanol extraction.
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis (tuber or seed), be ground into granule, or section;
(2) 85-95% ethanol percolation, preferred 90%, amount of alcohol be 12-30 doubly, preferred 18 times, the time is 12-48 hour, preferred 24 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 6-10 times of water gaging, 85-95 ℃, extract each 0.5-2 hour 2-4 time; 8 times of water gagings of preferred adding, extract each 1 hour 3 times by 90 ℃;
(5) filtered while hot, extracting solution added the 0.2-0.6% activated carbon decolorizing 2-12 hour, preferred 0.5%, 4 hour, under the room temperature, filtered carbon removal;
(6) be concentrated into the 5-15% of original volume, add the 90-100% alcohol chromatography, make to contain the alcohol amount and reach 75-85%; Preferably be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain alcohol amount and reach 80%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis.
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds water 4-10 times water, reflux, extract, 2-4 time, each 0.5-2 hour; 5 times of water gagings of preferred adding extract each 1.5 hours 3 times;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.2-1.5g, preferred 1.4g/ml;
(4) precipitate with ethanol is to containing alcohol amount 75-85%, preferred 80%; Time is 10-24 hour, preferred 12 hours;
(5) filter, it is 6.5-7.2 that filtrate is transferred pH, preferred 7.0, preferably uses 10% sodium hydroxide solution, or ammonia;
(6) leave standstill 10-24 hour, preferred 12 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract of the present invention.
The most preferred preparation method of the present invention in an embodiment.
The present invention also provides the pharmaceutical composition that is prepared into as active constituents of medicine with extract of the present invention, and pharmaceutical composition of the present invention comprises extract, and said composition can also add the medicine acceptable carrier as required.
Compositions of the present invention is the pharmaceutical dosage forms of unit dose, and described unit dosage form refers to the unit of preparation, such as every of tablet, and every capsules of capsule, every bottle of oral liquid, every bag of granule etc.
Compositions of the present invention active component wherein, its shared percentage by weight in preparation can be 0.1-99.9%, all the other are the medicine acceptable carrier.
Compositions of the present invention obtains by above-mentioned active component and medicine acceptable carrier are mixed with.
Compositions of the present invention, its pharmaceutical dosage forms can be any pharmaceutically useful dosage form, and these dosage forms comprise: tablet, sugar coated tablet, film coated tablet, enteric coated tablet, capsule, hard capsule, soft capsule, oral liquid, suck agent, granule, electuary, pill, powder, unguentum, sublimed preparation, suspensoid, powder, solution, injection, suppository, ointment, plaster, cream, spray, drop, patch.Preparation of the present invention, preferably injection, more preferably freeze-dried powder.
Compositions of the present invention, the preparation of its oral administration can contain excipient commonly used, such as binding agent, filler, diluent, tablet agent, lubricant, disintegrating agent, coloring agent, flavoring agent and wetting agent, can carry out coating to tablet in case of necessity.
Applicable filler comprises cellulose, mannitol, lactose and other similar filler.Suitable disintegrating agent comprises starch, polyvinylpyrrolidone and starch derivatives, for example sodium starch glycollate.Suitable lubricant comprises, for example magnesium stearate.The suitable acceptable wetting agent of medicine comprises sodium lauryl sulphate.
Can fill by mixing, the method that tabletting etc. are commonly used prepares solid oral composition.Repeatedly mix active substance is distributed in those compositionss of a large amount of filleies of whole use.
The form of oral liquid for example can be aqueous or oily suspensions, solution, Emulsion, syrup or elixir, perhaps can be a kind of before use available water or other suitable composite dry products of carrier.This liquid preparation can contain conventional additive, such as suspending agent, for example sorbitol, syrup, methylcellulose, gelatin, hydroxyethyl-cellulose, carboxymethyl cellulose, aluminium stearate gel or hydrogenation edible fat, emulsifying agent, for example lecithin, anhydro sorbitol monooleate or arabic gum; Non-aqueous carrier (they can comprise edible oil), for example almond oil, fractionated coconut oil, such as oily ester, propylene glycol or the ethanol of the ester of glycerol; Antiseptic, for example para hydroxybenzene methyl ester or propyl p-hydroxybenzoate or sorbic acid, and if necessary, can contain conventional flavouring agent or coloring agent.
For injection, the liquid unit dosage forms of preparation contains active substance of the present invention and sterile carrier.According to carrier and concentration, this chemical compound can be suspended or dissolving.The preparation of solution is normally by being dissolved in active substance in a kind of carrier filter-sterilized before it is packed into a kind of suitable bottle or ampoule, then sealing.Adjuvant for example a kind of local anesthetic, antiseptic and buffer agent also can be dissolved in this carrier.In order to improve its stability, can be after the bottle of packing into that this compositions is freezing, and under vacuum, water is removed.
Compositions of the present invention, when being prepared into medicament, optionally add suitable medicine acceptable carrier, described medicine acceptable carrier is selected from: meglumine, mannitol, sorbitol, sodium pyrosulfite, sodium sulfite, sodium thiosulfate, cysteine hydrochloride, TGA, methionine, vitamin C, EDETATE SODIUM, Ethylenediaminetetraacetic Acid Calcium Salt, the alkali-metal carbonate of monovalence, acetate, phosphate or its aqueous solution, hydrochloric acid, acetic acid, sulphuric acid, phosphoric acid, aminoacid, sodium chloride, potassium chloride, sodium lactate, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, mannitol, silicon derivative, cellulose and derivant thereof, alginate, gelatin, polyvinylpyrrolidone, glycerol, POLYSORBATE 80, agar, calcium carbonate, calcium bicarbonate, surfactant, Polyethylene Glycol, cyclodextrin, beta-schardinger dextrin-, the phospholipid material, Kaolin, Pulvis Talci, calcium stearate, magnesium stearate etc.
Compositions of the present invention is determined usage and dosage according to patient's situation in use, but takes every day three times, each 1-20 agent, as: 1-20 bag or grain or sheet.
Beneficial effect of the present invention:
By extracting method of the present invention, can obtain simultaneously Radix Ginseng extractum content 45-55%, preferred 50%, saponin content 4-5%, preferred 4.13%.
Concentrated Radix Ophiopogonis extractum, extract is Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, yield 54-62%, preferred 59%.
The total content of schisandrin B and schisandrin is 9.18-12.87%, preferred 9.98%.
(polysaccharide determination adopts: the phenolsulfuric acid method, like civilian extraction and the assay kind subworld 2004 that waits seed polysaccharide Radix Ophiopogonis, 12:24-26 referring to Zhao Hongqiao Zhu Jiong ripple Dong; Deoxyschizandrin and schisandrin B content assaying method referring to: Wang Ru Zhang Yancheng builds the preferred south China national defence medical journal 2006,19 (6) of the schisandra active component extraction processes such as peak: 4-6,47)
Solution stability testing:
With embodiment 1,2 or 3 extract, add meglumine; 100 ℃ were heated 1 hour, and cold preservation is spent the night, and added mannitol, filtered standardize solution; Get solution 2ml, canned transparent ampulla, sealing, the solution lucifuge is placed, and at 1 day, 3 days, 10 days, 30 days range estimation clarity the results are shown in following table.
Table 1 solution stability testing
Extracting method effective component extraction rate of the present invention is high, and cost is low, and is simple to operate, and finished product stability is good, and dosage is few, and curative effect is high, and instant effect is easy to long-time preservation.
The Concrete facts mode:
Further describe flesh and blood of the present invention below in conjunction with embodiments of the invention, this embodiment only is used for explanation the present invention and the present invention is not limited.
Embodiment 1
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 6 times of amount aquiferous ethanol, aquiferous ethanol concentration 40% was soaked 10 hours;
(3) boil extraction 2 times, each 2 hours, extracting solution merged;
(4) decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, adds 70% ethanol, and cold preservation 12 hours is filtered, and is concentrated, gets extractum, and obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
Make a living 18 times of dose of (2) 90% ethanol percolations, amount of alcohol, the time is 24 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 8 times of water gagings, 90 ℃, extract each 1 hour 3 times;
(5) filtered while hot, extracting solution add 0.5% activated carbon decolorizing 4 hours, under the room temperature, filter carbon removal;
(6) be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain alcohol amount and reach 80%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 5 times of water of water, reflux, extract, 3 times, each 1.5 hours;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.4g;
(4) precipitate with ethanol is to containing alcohol amount 80%; Time is 12 hours;
(5) filter, it is 7.0 that 10% sodium hydroxide solution is transferred pH;
(6) leave standstill 12 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
Embodiment 2
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) coarse powder is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 10 times of amount aquiferous ethanol, aquiferous ethanol concentration is preferred 10%, to soak 5 hours;
(3) boil extraction 1 time, each 1 hour, extracting solution merged;
(4) decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, and adding concentration is 50% ethanol, can cold preservation 8 hours, filter, and concentrated, get extractum, obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) section Radix Ophiopogonis;
(2) 85% ethanol percolations, amount of alcohol are 12 times, and the time is 12 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 6 times of water gagings, 85 ℃, extract each 0.5 hour 2 times;
(5) filtered while hot, extracting solution add 0.2% activated carbon decolorizing 2 hours, filter carbon removal;
(6) be concentrated into 5% of original volume, add 90% alcohol chromatography, make to contain alcohol amount and reach 75%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis.
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 4 times of water of water, reflux, extract, 2 times, each 0.5 hour;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.2g;
(4) precipitate with ethanol, to containing alcohol amount 75%, the time is 10 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution is 6.5;
(6) leave standstill 10 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract of the present invention.
Embodiment 3
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 8 times of amount aquiferous ethanol, aquiferous ethanol concentration 70% was soaked 12 hours;
(3) boil extraction 5 times, each 3 hours, extracting solution merged;
(4) decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, and adding concentration is 80% ethanol, can cold preservation 15 hours, filter, and concentrated, get extractum, obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis powder is broken into granule;
(2) 95% ethanol percolations, amount of alcohol are 30 times, and the time is 48 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 10 times of water gagings, 95 ℃, extract each 2 hours 4 times;
(5) filtered while hot, extracting solution add 0.6% activated carbon decolorizing 12 hours, filter carbon removal;
(6) be concentrated into 15% of original volume, add 100% alcohol chromatography, make to contain alcohol amount and reach 85%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 10 times of water of water, reflux, extract, 4 times, each 2 hours;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.5g;
(4) precipitate with ethanol, to containing alcohol amount 85%, the time is 24 hours;
(5) filter, transferring pH with ammonia is 7.2;
(6) leave standstill 24 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract of the present invention.
Embodiment 4
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 6 times of amount aquiferous ethanol, aquiferous ethanol concentration 40% was soaked 10 hours;
(3) boil extraction 2 times, each 2 hours, extracting solution merged;
(4) decolour by alumina column;
(5) concentrate to get extractum behind the n-butanol extraction, obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
Make a living 18 times of dose of (2) 90% ethanol percolations, amount of alcohol, the time is 24 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 8 times of water gagings, 90 ℃, extract each 1 hour 3 times;
(5) filtered while hot, extracting solution add 0.5% activated carbon decolorizing 4 hours, filter carbon removal;
(6) be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain alcohol amount and reach 80%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 5 times of water of water, reflux, extract, 3 times, each 1.5 hours;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.4g;
(4) precipitate with ethanol is to containing alcohol amount 80%; Time is 12 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution is 7.0;
(6) leave standstill 12 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
Embodiment 5
The preparation of lyophilized formulations:
(1) with embodiment 1,2,3 or 4 extract, adds meglumine; 100 ℃ were heated 1 hour, and cold preservation is spent the night, and added mannitol, filtered standardize solution;
(2) activated carbon decolorizing;
(3) moisturizing;
(4) aseptic filtration;
(5) fill;
(6) lyophilizing.
Embodiment 6
The preparation of other preparations:
With embodiment 1,2,3 or 4 extract, purchase into tablet according to the galenic pharmacy routine techniques, capsule, granule, the dosage forms such as oral liquid.
Claims (10)
1. the preparation method of a Yiqi and vein recovery extract, described Yiqi and vein recovery extract be by 1 part of Radix Ginseng, and 3 parts of Radix Ophiopogonis, 1.5 parts of Fructus Schisandrae Chinensis are made, and it is characterized in that described preparation method comprises:
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule or coarse powder are cut into slices, are ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 6-10 and doubly measure aquiferous ethanol, aquiferous ethanol concentration 10-70%;
(3) boil extraction 1-5 time, each 1-3 hour, extracting solution merged;
(4) decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, adds ethanol, and making determining alcohol is 50-80%, and cold preservation 8～15 hours is filtered, and is concentrated, gets extractum, and obtaining product is that the Radix Ginseng list is carried thing;
Wherein step 5 also can be with concentrating to get extractum behind the n-butanol extraction;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) be ground into granule Radix Ophiopogonis, or section;
(2) 85-95% ethanol percolation, amount of alcohol are 12-30 times, and the time is 12-48 hour, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 6-10 times of water gaging, 85-95 ℃, extract each 0.5-2 hour 2-4 time;
(5) filtered while hot, extracting solution added the 0.2-0.6% activated carbon decolorizing 2-12 hour, filtered carbon removal;
(6) be concentrated into the 5-15% of original volume, add the 90-100% alcohol chromatography, make to contain the alcohol amount and reach 75-85%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds water 4-10 times water, reflux, extract, 2-4 time, each 0.5-2 hour;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.2-1.5g;
(4) precipitate with ethanol, to containing alcohol amount 75-85%, the time is 10-24 hour;
(5) filter, it is 6.5-7.2 that filtrate is transferred pH, preferably uses 10% sodium hydroxide solution, or ammonia;
(6) leave standstill 10-24 hour;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
2. preparation method claimed in claim 1 is characterized in that,
The extracting method that described Radix Ginseng list is carried:
Wherein step (2) adds 6 times of amount aquiferous ethanol, aquiferous ethanol concentration 40%;
It is 1.14-1.16 that step (5) is concentrated into relative density, adds ethanol, and making determining alcohol is 70%, and cold preservation 12 hours is filtered, and concentrates, and gets extractum, or to get extractum with concentrating behind the n-butanol extraction,
The extracting method that singly carry described Radix Ophiopogonis,
Step (2) 90% ethanol percolations, amount of alcohol is 18 times, the time is 24 hours, defat;
Step (4) adds 8 times of water gagings, 90 ℃, extracts each 1 hour 3 times;
Step (5) filtered while hot, extracting solution adds 0.5% activated carbon decolorizing 4 hours, under the room temperature, filters carbon removal;
Step (6) is concentrated into original volume 10%, adds 95% alcohol chromatography, makes to contain alcohol amount and reach 80%:
The extracting method that described Fructus Schisandrae Chinensis list is carried,
Wherein step (1) schisandra chinensis medicinal material adds 5 times of water gagings, extracts each 1.5 hours 3 times;
Step (3) filtrate is concentrated into every milliliter contained material 1.4g;
Step (4) precipitate with ethanol, to containing alcohol amount 80%, the time is 12 hours;
Step (5) is filtered, and transferring pH with 10% sodium hydroxide solution or ammonia is 7.0;
Step (6) left standstill 12 hours.
3. preparation method claimed in claim 1 is characterized in that,
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 6 times of amount aquiferous ethanol, aquiferous ethanol concentration 40% was soaked 10 hours;
(3) boil extraction 2 times, each 2 hours, extracting solution merged;
(4) decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, adds 70% ethanol, and cold preservation 12 hours is filtered, and is concentrated, gets extractum, and obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
Make a living 18 times of dose of (2) 90% ethanol percolations, amount of alcohol, the time is 24 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 8 times of water gagings, 90 ℃, extract each 1 hour 3 times;
(5) filtered while hot, extracting solution add 0.5% activated carbon decolorizing 4 hours, under the room temperature, filter carbon removal;
(6) be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain alcohol amount and reach 80%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 5 times of water of water, reflux, extract, 3 times, each 1.5 hours;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.4g;
(4) precipitate with ethanol is to containing alcohol amount 80%; Time is 12 hours;
(5) filter, it is 7.0 that 10% sodium hydroxide solution is transferred pH;
(6) leave standstill 12 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
4. preparation method claimed in claim 1 is characterized in that,
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) coarse powder is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 10 times of amount aquiferous ethanol, aquiferous ethanol concentration 10% was soaked 5 hours;
(3) boil extraction 1 time, each 1 hour, extracting solution merged;
(4) decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, and adding concentration is 50% ethanol, can cold preservation 8 hours, filter, and concentrated, get extractum, obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) section Radix Ophiopogonis;
(2) 85% ethanol percolations, amount of alcohol are 12 times, and the time is 12 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 6 times of water gagings, 85 ℃, extract each 0.5 hour 2 times;
(5) filtered while hot, extracting solution add 0.2% activated carbon decolorizing 2 hours, filter carbon removal;
(6) be concentrated into 5% of original volume, add 90% alcohol chromatography, make to contain alcohol amount and reach 75%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 4 times of water of water, reflux, extract, 2 times, each 0.5 hour;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.2g;
(4) precipitate with ethanol, to containing alcohol amount 75%, the time is 10 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution is 6.5;
(6) leave standstill 10 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
5. preparation method claimed in claim 1 is characterized in that,
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 8 times of amount aquiferous ethanol, aquiferous ethanol concentration 70% was soaked 12 hours;
(3) boil extraction 5 times, each 3 hours, extracting solution merged;
(4) decolour by alumina column;
(5) being concentrated into relative density is 1.14-1.16, and adding concentration is 80% ethanol, and cold preservation 15 hours is filtered, and is concentrated, gets extractum, and obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis powder is broken into granule;
(2) 95% ethanol percolations, amount of alcohol are 30 times, and the time is 48 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 10 times of water gagings, 95 ℃, extract each 2 hours 4 times;
(5) filtered while hot, extracting solution add 0.6% activated carbon decolorizing 12 hours, filter carbon removal;
(6) be concentrated into 15% of original volume, add 100% alcohol chromatography, make to contain alcohol amount and reach 85%;
(7) concentrate to get extractum, for singly carrying thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 10 times of water of water, reflux, extract, 4 times, each 2 hours;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.5g;
(4) precipitate with ethanol, to containing alcohol amount 85%, the time is 24 hours;
(5) filter, transferring pH with ammonia is 7.2;
(6) leave standstill 24 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
6. preparation method claimed in claim 1 is characterized in that,
(1) the Radix Ginseng list is carried, and extraction step is as follows:
(1) granule is cut into slices, is ground into to fibrous root of Radix Ginseng coarse powder, Radix Ginseng;
(2) add 6 times of amount aquiferous ethanol, aquiferous ethanol concentration 40% was soaked 10 hours;
(3) boil extraction 2 times, each 2 hours, extracting solution merged;
(4) decolour by alumina column;
(5) concentrate to get extractum behind the n-butanol extraction, obtaining product is that the Radix Ginseng list is carried thing;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
Make a living 18 times of dose of (2) 90% ethanol percolations, amount of alcohol, the time is 24 hours, defat;
(3) dry alcohol Radix Ophiopogonis behind the percolation;
(4) add 8 times of water gagings, 90 ℃, extract each 1 hour 3 times;
(5) filtered while hot, extracting solution add 0.5% activated carbon decolorizing 4 hours, filter carbon removal;
(6) be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain alcohol amount and reach 80%;
(7) concentrate to get extractum, be Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, obtaining product is singly to carry thing Radix Ophiopogonis;
(3) the Fructus Schisandrae Chinensis list is carried, and extraction step is as follows:
(1) schisandra chinensis medicinal material adds 5 times of water of water, reflux, extract, 3 times, each 1.5 hours;
(2) extracting solution merges, and filters;
(3) filtrate is concentrated into every milliliter contained material 1.4g;
(4) precipitate with ethanol is to containing alcohol amount 80%; Time is 12 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution is 7.0;
(6) leave standstill 12 hours;
(7) filter, concentrated, drying, obtaining product is that the Fructus Schisandrae Chinensis list is carried thing;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
7. the Yiqi and vein recovery extract for preparing with any one preparation method of claim 1-6.
8. the pharmaceutical composition that contains extract claimed in claim 7.
9. pharmaceutical composition claimed in claim 8 is injection.
10. pharmaceutical composition claimed in claim 9 is freeze-dried powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810153789 CN101745008B (en) | 2008-12-05 | 2008-12-05 | Extraction method of ginseng, ophiopogon root and shiandra and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810153789 CN101745008B (en) | 2008-12-05 | 2008-12-05 | Extraction method of ginseng, ophiopogon root and shiandra and preparation thereof |
Publications (2)
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| CN101874869A (en) * | 2009-04-28 | 2010-11-03 | 河北以岭医药研究院有限公司 | Method for measuring loganin content of Chinese medicinal composition |
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| CN101310751A (en) * | 2007-05-23 | 2008-11-26 | 北京亚东生物制药有限公司 | Traditional Chinese medicine composition for replenishing qi and blood, preparation method and quality control method thereof |
| CN101874869A (en) * | 2009-04-28 | 2010-11-03 | 河北以岭医药研究院有限公司 | Method for measuring loganin content of Chinese medicinal composition |
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| 郑天孝.生脉注射液的工业制备.《华西药学杂志》.1987,(第03期), * |
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