CN101745010A - 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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- CN101745010A CN101745010A CN200810153794A CN200810153794A CN101745010A CN 101745010 A CN101745010 A CN 101745010A CN 200810153794 A CN200810153794 A CN 200810153794A CN 200810153794 A CN200810153794 A CN 200810153794A CN 101745010 A CN101745010 A CN 101745010A
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- China
- Prior art keywords
- water
- thing
- ethanol
- fructus schisandrae
- schisandrae chinensis
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Landscapes
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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 Chinese medicine extraction method and pharmaceutical preparation thereof, particularly a kind of qi-tonifying and pulse-restoring preparation for the treatment of cardiovascular disease and preparation method thereof, said preparation are by Radix Ginseng, and Radix Ophiopogonis and Fructus Schisandrae Chinensis three flavor Chinese medicines are prepared from.
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, 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.Fruit of Fructus Schisandrae Chinensis is made Chinese medicine function supplementing QI for promoting the production of body fluid, the nourishing kidney of astringing the lung, antidiarrheal, arresting seminal emission, is calmed the nerves, and can control 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 the reduction 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 is formed, 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 that injection is given birth to the arteries and veins lyophilized injectable powder for preparing, earlier to Fructus Schisandrae Chinensis 60-80% alcohol reflux 2-3 time, each 60-120min, reclaim ethanol 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; Fructus Schisandrae Chinensis medicinal residues and Radix Ginseng behind the reuse ethanol extraction, adding hydration Radix Ophiopogonis fries in shallow oil, after the merging aqueous extract concentrates,, filter again through precipitate with ethanol, reclaim behind the ethanol doubly measure deionized water dissolving with 10-15 after, handle with macroporous adsorbent resin, be washed till sugar-free with deionized water earlier, be washed till no Saponin with ethanol again and end, reclaim alcohol eluen, concentrate extracting solution B; With above-mentioned Radix Ginseng, the precipitation adding distil water behind Radix Ophiopogonis and the Fructus Schisandrae Chinensis water extract-alcohol precipitation dissolves, and filters, and drying gets water and carries 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 to remove upper strata oil, filter, concentrate, 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 concentrates, and 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, and the Radix Ginseng Rubra ethanol extraction reclaims ethanol, and aqueous precipitation filters, and concentrates, and vacuum drying, spray drying or lyophilization get Radix Ginseng Rubra extract; Radix Ophiopogonis, Fructus Schisandrae Chinensis water extraction, after extracting solution concentrated, precipitate with ethanol reclaimed ethanol, and medicinal liquid is concentrated, and reuse vacuum drying, spray drying or freeze-drying drying 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 CN 200310121126.6 discloses a kind of injection and has given birth to arteries and veins 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 ethanol to ooze the source earlier and extracts, and gets Radix Ginseng Rubra extracts active ingredients liquid a; To ooze the Radix Ginseng Rubra reuse alcohol reflux that extracted in the source subsequently, 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 filtrate concentrates the back precipitate with ethanol, gets supernatant then and filters, filtrate and above-mentioned a, b merge, and cold preservation is got supernatant and filtered, filtrate concentrates the back water precipitating, gets supernatant then and filters, and promptly gets the medicinal component extracting solution of Radix Ginseng Rubra C; (2) adopt alcohol reflux Radix Ophiopogonis earlier, cold preservation is got supernatant and is filtered, and filtrate concentrates the back water precipitating, gets supernatant again and filters, and promptly gets extracts active ingredients liquid d Radix Ophiopogonis; Use water boiling and extraction again the Radix Ophiopogonis that alcohol reflux is crossed, filter, filtrate concentrates the back precipitate with ethanol, get supernatant then and filter, reclaim ethanol and be concentrated into thick paste shape, water precipitating, getting supernatant then filters, promptly get medicinal component extracting solution e Radix Ophiopogonis: extracts active ingredients liquid d and e merge with Radix Ophiopogonis, filter, and promptly get medicinal component extracting solution f Radix Ophiopogonis; (3) the Fructus Schisandrae Chinensis distillate adopts the Fructus Schisandrae Chinensis steam distillation, collect distillate and promptly get Fructus Schisandrae Chinensis distillate g: the Fructus Schisandrae Chinensis behind the collection distillate adopts alcohol reflux earlier, cold preservation, getting supernatant filters, filter and concentrate the back water precipitating, getting supernatant filters, promptly get Fructus Schisandrae Chinensis extracts active ingredients liquid h: the Fructus Schisandrae Chinensis water boiling and extraction of again alcohol reflux being crossed, filter, filtrate concentrates back secondary precipitate with ethanol, gets supernatant then and filters, reclaim ethanol and be concentrated into the thick paste shape, water precipitating goes supernatant to filter then, promptly 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, promptly get the medicinal composition extracting solution of Fructus Schisandrae Chinensis j.
Chinese patent CN99114091.5 discloses medicine of a kind of cardiovascular diseases of treatment 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 CN 200510088087.3 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, cold slightly filtration, this technology 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 decocting in water precipitate 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 technology 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 and uses 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 and uses 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, liquor C is used for dosing; With filtrate A, B, C mixing, make different preparations according to conventional method.
Complex manufacturing in the prior art, the cost height, the problem that extraction ratio is low never is overcome.
The present invention has overcome the shortcoming of existing extraction process through research for a long time, has invented a kind of effective component extraction rate height, 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 together to be extracted two flavor Chinese medicines in 1 part of Radix Ginseng, 3 parts of Radix Ophiopogonis, 1.5 part of three flavor of the Fructus Schisandrae Chinensis Chinese medicine, and another Chinese medicine extracts separately.
Preparation method of the present invention is with Fructus Schisandrae Chinensis, closes Radix Ophiopogonis and carries, and the Radix Ginseng list is carried.
Preparation method of the present invention, wherein said close to carry be meant that with Radix Ophiopogonis, Fructus Schisandrae Chinensis mixes.With water extraction or use alcohol extraction.Described singly carrying is meant Radix Ginseng extracted separately with water extraction or with alcohol extraction.
Wherein be meant to be soaked in water or water heating is boiled and carried or the water heating and refluxing extraction with water extraction,
Be meant that with alcohol extraction using the solvent that contains ethanol or other alcohols materials to use soaks, percolation, 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, methods such as recrystallization.
For this reason, preparation method of the present invention preferably adopts following method
(1) Radix Ophiopogonis, Fructus Schisandrae Chinensis close that to carry extraction step as follows:
(1) gets the Radix Ophiopogonis and the Fructus Schisandrae Chinensis of recipe quantity, water boiling and extraction;
(2) collect the water extract, supernatant is collected in precipitate with ethanol, filtration;
(3) residue is with 85～95% alcohol reflux;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing.
Wherein
Step (1) is that the water of 4～10 times of water backflows refluxes each 30 minutes to 2 hours 2～3 times.
Step (2) is the ethanol precipitation with 85～95%, and cold preservation is filtered.
Step (3) is with 4～10 times alcohol reflux 2～3 times, each 30 minutes to 2 hours.
(2) the Radix Ginseng list is carried, and extraction step is as follows:
The Radix Ginseng section, the alcohol reflux with 50～95% behind the recovery ethanol, adopts macroporous adsorbent resin method purification.Wherein:
Alcohol reflux 2～4 times, each 1～3 hour.
Macroporous resin is selected from D101 resin or D4020 resin.
When selecting the D101 resin for use, first water is removed impurity, uses 30～90% ethanol elution then, preferably uses 3 column volumes of 70% ethanol elution, merges eluent, concentrates, and filters, and the reconcentration drying is singly carried thing.
When selecting the D4020 resin for use, wash with water earlier to colourless, 2% alkali liquor eluting impurity, washing, reuse 90% ethanol is washed, and merges eluent, concentrates, and filters, and the reconcentration drying is singly carried thing.
More than close to carry thing and singly propose the thing merging and be 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 is meant the unit of preparation, as every of tablet, and capsular every capsules, 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.
The filler that is suitable for 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 acceptable wetting agent of appropriate drug comprises sodium lauryl sulphate.
Can fill by mixing, the method that tabletting etc. are commonly used prepares solid oral composition.Mix repeatedly 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 available water before use 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 desired, 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, sealing then.For example a kind of local anesthetic of adjuvant, 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, the EDTA disodium, EDTA calcium sodium, 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, soil temperature 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 obeys 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 Fructus Schisandrae Chinensis lignanoid and Radix Ophiopogonis polysaccharide simultaneously, polyoses content is about 3.8-4%, and deoxyschizandrin and schisandrin B content are more than 10%, and impurity is few.
The Radix Ginseng total saponins eluting rate is more than 90%, and Radix Ginseng total saponins content is about 60% in the purity height, dry extract behind the purification (powder), and refining degree reaches more than 200%; Ginsenoside's purification rate 2.5%, minimum extractum rate 54.7%.
(polysaccharide determination adopts: the phenolsulfuric acid method, like the extraction and the assay kind subworld 2004 of seed polysaccharide Radix Ophiopogonis such as literary composition, 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 schisandra active component extraction processes such as peak: 4-6,47)
Solution stability testing:
With the extract of embodiment 1,2 or 3, 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 peace bottle, 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 height of the present invention, cost is low, and is simple to operate, and finished product stability is good, and dosage is few, the curative effect height, instant effect is easy to long-time preservation.
Concrete true mode:
Further describe flesh and blood of the present invention below in conjunction with embodiments of the invention, this embodiment only is used to the present invention is described and the present invention is not limited.
Embodiment 1
(1) Radix Ophiopogonis, Fructus Schisandrae Chinensis close and carry, and extraction step is as follows:
(1) get Radix Ophiopogonis and Fructus Schisandrae Chinensis, the water that the water backflow is 4 times refluxes each 30 minutes 2 times;
(2) collect the water extract, the ethanol precipitation with 85%, cold preservation is filtered, and collects supernatant;
(3) residue was with 85% alcohol reflux of 4 times of amounts 2 times, each 30 minutes;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing;
(2) the Radix Ginseng list is carried, and extraction step is as follows:
The Radix Ginseng section, the alcohol reflux with 50% 2 times, each 1 hour, behind the recovery ethanol, select D101 resin chromatography for use, first water is removed impurity, uses 30% ethanol elution then, 3 column volumes of eluting, merge eluent, concentrate, filter, the reconcentration drying is singly carried thing.
More than close to carry thing and singly propose the thing merging and be extract of the present invention.
Embodiment 2
(1) Radix Ophiopogonis, Fructus Schisandrae Chinensis close and carry, and extraction step is as follows:
(1) get Radix Ophiopogonis and Fructus Schisandrae Chinensis, water refluxes, and 10 times water refluxes 3 times, each 2 hours;
(2) collect the water extract, the ethanol precipitation with 90%, cold preservation is filtered, and collects supernatant;
(3) residue was with 90% alcohol reflux of 4 times of amounts 3 times, each 1 hour;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing;
(2) the Radix Ginseng list is carried, and extraction step is as follows:
The Radix Ginseng section, the alcohol reflux with 95% 4 times each 3 hours, behind the recovery ethanol, is selected D4020 resin chromatography for use, wash with water earlier to colourless, 2% alkali liquor eluting impurity, washing, reuse 90% ethanol is washed, merge eluent, concentrate, filter, the reconcentration drying is singly carried thing.
More than close to carry thing and singly propose the thing merging and be extract of the present invention.
Embodiment 3
(1) Radix Ophiopogonis, Fructus Schisandrae Chinensis close and carry, and extraction step is as follows:
(1) get Radix Ophiopogonis and Fructus Schisandrae Chinensis, water refluxes, and the water of 6 times of amounts refluxes 3 times, each 1 hour;
(2) collect the water extract, the ethanol precipitation with 95%, cold preservation is filtered, and collects supernatant;
(3) residue was with 95% alcohol reflux of 4 times of amounts 3 times, each 2 hours;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing;
(2) the Radix Ginseng list is carried, and extraction step is as follows:
The Radix Ginseng section, the alcohol reflux with 75% 3 times, each 2 hours, behind the recovery ethanol, when selecting the D101 resin for use, first water was removed impurity, and 3 column volumes of 70% ethanol elution merge eluent then, concentrate, and filter, and the reconcentration drying is singly carried thing.
More than close to carry thing and singly propose the thing merging and be extract of the present invention.
Embodiment 4
The preparation of lyophilized formulations:
(1) with the extract of embodiment 1,2 or 3, 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 5
The preparation of other preparations:
With the extract of embodiment 1,2,3 or 4, purchase into tablet according to the galenic pharmacy routine techniques, capsule, granule, dosage forms such as oral liquid.
Claims (10)
1. Yiqi and vein recovery preparation method of extract, described Yiqi and vein recovery extract is by 1 part of Radix Ginseng, and 3 parts of Radix Ophiopogonis, Fructus Schisandrae Chinensis is made for 1.5 parts, it is characterized in that, and described preparation method comprises:
Radix Ophiopogonis, Fructus Schisandrae Chinensis close to be carried, and extraction step is as follows:
(1) gets Radix Ophiopogonis and Fructus Schisandrae Chinensis, water boiling and extraction;
(2) collect the water extract, supernatant is collected in precipitate with ethanol, filtration;
(3) residue is with 85～95% alcohol reflux;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing,
The Radix Ginseng list is carried, and extraction step is as follows:
Radix Ginseng is with 50～95% alcohol reflux, reclaim ethanol after, adopt macroporous adsorbent resin method purification, singly carried thing; Close to carry thing and singly propose the thing merging and obtain extract.
2. the described preparation method of claim 1 is characterized in that, described Radix Ophiopogonis, Fructus Schisandrae Chinensis close the extracting method of carrying, wherein
Step (1) is that the water of 4～10 times of water backflows refluxes each 30 minutes to 2 hours 2～3 times;
Step (2) is the ethanol precipitation with 85～95%, and cold preservation is filtered;
Step (3) is with 4～10 times alcohol reflux 2～3 times, each 30 minutes to 2 hours.
3. the described preparation method of claim 1 is characterized in that,
Radix Ophiopogonis, Fructus Schisandrae Chinensis close to be carried, and extraction step is as follows:
(1) get Radix Ophiopogonis and Fructus Schisandrae Chinensis, the water that the water backflow is 4 times refluxes each 30 minutes 2 times;
(2) collect the water extract, the ethanol precipitation with 85%, cold preservation is filtered, and collects supernatant;
(3) residue was with 85% alcohol reflux of 4 times of amounts 2 times, each 30 minutes;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing;
The Radix Ginseng list is carried, and extraction step is as follows:
The Radix Ginseng section, the alcohol reflux with 50% 2 times, each 1 hour, after reclaiming ethanol, select D101 resin chromatography for use, first water is removed impurity, uses 30% ethanol elution then, 3 column volumes of eluting, merge eluent, concentrate, filter, the reconcentration drying is singly carried thing, closes to carry thing and singly propose the thing merging to obtain extract.
4. the described preparation method of claim 1 is characterized in that,
Radix Ophiopogonis, Fructus Schisandrae Chinensis close to be carried, and extraction step is as follows:
(1) get Radix Ophiopogonis and Fructus Schisandrae Chinensis, water refluxes, and 10 times water refluxes 3 times, each 2 hours;
(2) collect the water extract, the ethanol precipitation with 90%, cold preservation is filtered, and collects supernatant;
(3) residue was with 90% alcohol reflux of 4 times of amounts 3 times, each 1 hour;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing;
The Radix Ginseng list is carried, and extraction step is as follows:
The Radix Ginseng section, the alcohol reflux with 95% 4 times, each 3 hours, after reclaiming ethanol, select D4020 resin chromatography for use, wash with water earlier to colourless, 2% alkali liquor eluting impurity, washing, reuse 90% ethanol is washed, and merges eluent, concentrate, filter, the reconcentration drying is singly carried thing, closes to carry thing and singly propose the thing merging to obtain extract.
5. the described preparation method of claim 1 is characterized in that,
Radix Ophiopogonis, Fructus Schisandrae Chinensis close to be carried, and extraction step is as follows:
(1) get Radix Ophiopogonis and Fructus Schisandrae Chinensis, water refluxes, and the water of 6 times of amounts refluxes 3 times, each 1 hour;
(2) collect the water extract, the ethanol precipitation with 95%, cold preservation is filtered, and collects supernatant;
(3) residue was with 95% alcohol reflux of 4 times of amounts 3 times, each 2 hours;
(4) extracting solution of concentration step (2) and step (3) obtains closing and carries thing;
The Radix Ginseng list is carried, and extraction step is as follows:
The Radix Ginseng section, alcohol reflux with 75% 3 times, each 2 hours, behind the recovery ethanol, when selecting the D101 resin for use, elder generation's water is removed impurity, and 3 column volumes of 70% ethanol elution merge eluent then, concentrate, filter, the reconcentration drying is singly carried thing, closes to carry thing and singly propose the thing merging to obtain extract.
6. use the Yiqi and vein recovery extract of any one preparation method preparation of claim 1-5.
7. the pharmaceutical composition that contains the described extract of claim 6.
8. the described pharmaceutical composition of claim 7 is an injection.
9. the described pharmaceutical composition of claim 8 is a freeze-dried powder.
10. the described pharmaceutical composition of claim 9 adds the medicine acceptable carrier in case of necessity.
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