CN101744998B - 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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- CN101744998B CN101744998B CN 200810153779 CN200810153779A CN101744998B CN 101744998 B CN101744998 B CN 101744998B CN 200810153779 CN200810153779 CN 200810153779 CN 200810153779 A CN200810153779 A CN 200810153779A CN 101744998 B CN101744998 B CN 101744998B
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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, 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.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; 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 concentrates, again through precipitate with ethanol, filter, 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 dissolving behind Radix Ophiopogonis and the Fructus Schisandrae Chinensis water extract-alcohol precipitation 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 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 uses vacuum drying, spray drying or freeze-drying drying again, gets 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 that extracted in the source subsequently and use alcohol reflux again, 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 namely 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 namely 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, namely get medicinal component extracting solution e Radix Ophiopogonis: extracts active ingredients liquid d and e merge with Radix Ophiopogonis, filter, and 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 alcohol reflux earlier, cold preservation, getting supernatant filters, filter and concentrate the back 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, 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, 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, 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, get liquor C and use 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 that with 1 part of Radix Ginseng, 3 parts of Radix Ophiopogonis, 1.5 parts of Fructus Schisandrae Chinensis three flavor Chinese medicines extract separately, extract are mixed being prepared into preparation.
Described singly carrying refers to three flavor Chinese medicines are extracted separately with water extraction or with alcohol extraction respectively.
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, 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 or microwave 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) 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 6-12 and doubly measure moisture lower alcohol, preferred 8 times of amounts; Moisture concentration of lower alcohols is 10-98%,
Preferred 40-85%, further preferred 45-75%; Reflux, extract, 2-8 time each 0.5-8 hour, is preferably extracted each 3 hours 6 times; Lower alcohol is methanol, ethanol, is preferably ethanol;
(3) merge extractive liquid,, extracting solution concentrate extractum; Better elder generation is with n-butanol extraction before concentrating, and extract concentrates, and gets extractum; Best, before n-butanol extraction, can chloroform or dichloromethane defat;
(4) get extractum, obtain product and carry thing for the Radix Ginseng list;
(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, and preferred 0.5%, 4 hour, under the room temperature;
(6) filter carbon removal, 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 extractum, 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 ml and contains raw medicinal herbs 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, concentrate, drying obtains product and carries thing for the Fructus Schisandrae Chinensis list;
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, 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.
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.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, 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 the Radix Ginseng list simultaneously and carry thing, ginsenoside total rate of transform 87-93%, preferred 90.19%; Extractum content 42-47%, preferred 46%, brownish red bulk, saponin content 8.2-8.9%, preferred 8.57%; Radix Ophiopogonis polysaccharide and Radix Ophiopogonis total saponins, its yield 54-62%, general 59%; The total content of schisandrin B and schisandrin is 9.18-12.87%, optimum 9.98%.
(polysaccharide determination adopts: the phenolsulfuric acid method, like 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 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 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 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 8 times of moisture lower alcohols of amount, moisture concentration of lower alcohols is 60%, reflux, extract, 6 times, and each 3 hours, lower alcohol was ethanol;
(3) dichloromethane defat, n-butanol extraction, extract concentrate, merge extractive liquid,, extracting solution concentrate extractum, obtain product and carry thing for the Radix Ginseng list;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
(2) 90% ethanol percolations, amount of alcohol are 18 times, and 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;
(6) filter carbon removal, be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain the alcohol amount and reach 80%;
(7) concentrate extractum, 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 ml and contains raw medicinal herbs 1.4g;
(4) precipitate with ethanol, to containing alcohol amount 80%, the time is 12 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution is 7.0;
(6) leave standstill 12 hours;
(7) filter, concentrate, drying obtains product and carries thing for the Fructus Schisandrae Chinensis list;
The thing of singly carrying that merges above three kinds of medicines obtains extract of the present invention.
Embodiment 2
(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 moisture lower alcohols of amount, moisture concentration of lower alcohols is 60%; Reflux, extract, 6 times, each 3 hours, lower alcohol was for being ethanol;
(3) dichloromethane defat, n-butanol extraction, extract concentrate, merge extractive liquid,, extracting solution concentrate extractum, obtain product and carry thing for the Radix Ginseng list;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
(2) 90% ethanol percolations, amount of alcohol are 18 times, and 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;
(6) filter carbon removal, be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain the alcohol amount and reach 80%;
(7) concentrate extractum, 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 ml and contains raw medicinal herbs 1.2g/ml;
(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, concentrate, drying obtains product and carries thing for the Fructus Schisandrae Chinensis list;
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 6 times of moisture lower alcohols of amount, moisture concentration of lower alcohols is 45%, reflux, extract, 2 times, and each 0.5 hour, lower alcohol was methanol;
(3) merge extractive liquid,, extracting solution concentrate extractum, obtain product and carry thing for the Radix Ginseng list;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
(2) 85% ethanol percolations, amount of alcohol are 12, and the time is 128 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, under the room temperature;
(6) filter carbon removal, be concentrated into 5% of original volume, add 90% alcohol chromatography, make to contain the alcohol amount and reach 75%;
(7) concentrate extractum, 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 ml and contains raw medicinal herbs 1.5g;
(4) precipitate with ethanol, to containing alcohol amount 85%, the time is 24 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution is 7.2;
(6) leave standstill 24 hours;
(7) filter, concentrate, drying obtains product and carries thing for the Fructus Schisandrae Chinensis list;
The thing of singly carrying that merges above three kinds of medicines obtains extract of the present invention.
Embodiment 4
The preparation of lyophilized formulations:
(1) with embodiment 1,2 or 3 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, dosage forms such as oral liquid.
Claims (9)
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:
(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 6-12 and doubly measure moisture lower alcohol, moisture concentration of lower alcohols is 10-98%, reflux, extract, 2-8 time, and each 0.5-8 hour, lower alcohol was methanol, ethanol;
(3) merge extractive liquid,, extracting solution concentrate extractum, obtain product and carry thing for the Radix Ginseng list;
(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, under the room temperature;
(6) filter carbon removal, 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 extractum, 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 ml and contains raw medicinal herbs 1.2-1.5g;
(4) precipitate with ethanol, to containing alcohol amount 75-85%, the time is 10-24 hour;
(5) filter, transferring pH with 10% sodium hydroxide solution or ammonia is 6.5-7.2;
(6) leave standstill 10-24 hour;
(7) filter, concentrate, drying obtains product and carries thing for the Fructus Schisandrae Chinensis list;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
2. the described preparation method of claim 1 is characterized in that, the extracting method that described Radix Ginseng list is carried: wherein step (2) adds 8 times of moisture lower alcohols of amount, and moisture concentration of lower alcohols is 40-85%, reflux, extract, 2-8 time, and each 0.5-8 hour, lower alcohol was ethanol;
(3) chloroform or dichloromethane defat, n-butanol extraction, merge extractive liquid,, extracting solution concentrate extractum;
The extracting method that singly carry described Radix Ophiopogonis:
Step (2) 90% ethanol percolations wherein, amount of alcohol is 18 times, the time is 24 hours, defat;
(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;
(6) filter carbon removal, be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain the 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 of water, reflux, extract, 3 times, each 1.5 hours;
(3) filtrate is concentrated into every ml and contains raw medicinal herbs 1.4g;
(4) precipitate with ethanol, to containing alcohol amount 80%, the time is 12 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution or ammonia is 7.0;
(6) leave standstill 12 hours.
3. the described preparation method of 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 moisture lower alcohols of amount, moisture concentration of lower alcohols is 60%, reflux, extract, 6 times, and each 3 hours, lower alcohol was ethanol;
(3) dichloromethane defat, n-butanol extraction, extract concentrate, merge extractive liquid,, extracting solution concentrate extractum, obtain product and carry thing for the Radix Ginseng list;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
(2) 90% ethanol percolations, amount of alcohol are 18 times, and 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;
(6) filter carbon removal, be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain the alcohol amount and reach 80%;
(7) concentrate extractum, 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 ml and contains raw medicinal herbs 1.4g;
(4) precipitate with ethanol, to containing alcohol amount 80%, the time is 12 hours;
(5) filter, transferring pH with 10% sodium hydroxide solution is 7.0;
(6) leave standstill 12 hours;
(7) filter, concentrate, drying obtains product and carries thing for the Fructus Schisandrae Chinensis list;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
4. the described preparation method of 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 moisture lower alcohols of amount, moisture concentration of lower alcohols is 60%, reflux, extract, 6 times, and each 3 hours, lower alcohol was for being ethanol;
(3) dichloromethane defat, n-butanol extraction, extract concentrate, merge extractive liquid,, extracting solution concentrate extractum, obtain product and carry thing for the Radix Ginseng list;
(2) singly carry Radix Ophiopogonis, extraction step is as follows:
(1) Radix Ophiopogonis, is ground into granule;
(2) 90% ethanol percolations, amount of alcohol are 18 times, and 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;
(6) filter carbon removal, be concentrated into 10% of original volume, add 95% alcohol chromatography, make to contain the alcohol amount and reach 80%;
(7) concentrate extractum, 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 ml and contains raw medicinal herbs 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, concentrate, drying obtains product and carries thing for the Fructus Schisandrae Chinensis list;
The thing of singly carrying that merges above three kinds of medicines obtains extract.
5. use the Yiqi and vein recovery extract of any one preparation method preparation of claim 1-4.
6. the pharmaceutical composition that contains the described extract of claim 5.
7. the described pharmaceutical composition of claim 6 is injection.
8. the described pharmaceutical composition of claim 7 is freeze-dried powder.
9. the described pharmaceutical composition of claim 8 adds the medicine acceptable carrier in case of necessity.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1559564A (en) * | 2004-02-24 | 2005-01-05 | 贵州益佰制药股份有限公司 | Supplementing qi pulse restoring Chinese medicinal preparation and its preparation method |
| CN1814166A (en) * | 2005-12-02 | 2006-08-09 | 佟兵 | Pulse-promoting powder injecta and preparing method |
| CN1872278A (en) * | 2005-06-03 | 2006-12-06 | 天津天士力制药股份有限公司 | A composition of medication |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559564A (en) * | 2004-02-24 | 2005-01-05 | 贵州益佰制药股份有限公司 | Supplementing qi pulse restoring Chinese medicinal preparation and its preparation method |
| CN1872278A (en) * | 2005-06-03 | 2006-12-06 | 天津天士力制药股份有限公司 | A composition of medication |
| CN1814166A (en) * | 2005-12-02 | 2006-08-09 | 佟兵 | Pulse-promoting powder injecta and preparing method |
Non-Patent Citations (1)
| Title |
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| 吕丽娟等.正交实验法优选麦冬多糖提取工艺.《长春中医药大学学报》.2007,第23卷(第02期),30-31. * |
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