CN102895294A - Astragalus mongholicus injection and preparation method thereof - Google Patents
Astragalus mongholicus injection and preparation method thereof Download PDFInfo
- Publication number
- CN102895294A CN102895294A CN2012104224996A CN201210422499A CN102895294A CN 102895294 A CN102895294 A CN 102895294A CN 2012104224996 A CN2012104224996 A CN 2012104224996A CN 201210422499 A CN201210422499 A CN 201210422499A CN 102895294 A CN102895294 A CN 102895294A
- Authority
- CN
- China
- Prior art keywords
- injection
- alcohol
- water
- ethanol
- filter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to Astragalus mongholicus injection and a preparation method thereof. The injection contains two effective components: astragaloside and calycosin-7-glycoside. 1ml of Astragalus mongholicus injection contains 0.08-0.8mg of astragaloside and 0.02-0.4mg of calycosin-7-glycoside, wherein the astragaloside accounts for 1-10 percent of total solids, and the calycosin-7-glycoside accounts for 0.20-5 percent of the total solids. The injection provided by the invention is better in adjuvant therapeutic effect in the aspects of treating myocarditis, myocardial ischemia, cardiac failure, myocardial infarction and arrhythmia, and the therapeutic effect of the injection is superior to that of the prior art.
Description
Technical field
The present invention relates to the formulation of astragalus root field, be specifically related to a kind of Radix Astragali injection and preparation method thereof.
Background technology
The Radix Astragali is the root of leguminous herbaceous plant's Radix Astagali, Radix Astragali; existing pharmaceutical research confirms; the Radix Astragali has heart tonifying, vasodilative effect; and the Radix Astragali can improve cardiac diastolic function when improving cardiac systolic function; myocardium protecting action is still arranged except the heart failure effect; can protect hypoxic-ischemic, ischemia-reperfusion and infect the cardiac muscle of virus, and can improve the electrical activity of myocardial cell, and have the effect such as arteriosclerosis.
The chemical composition of the Radix Astragali mainly contains saponins, flavonoid, polysaccharide and amino acids etc., and wherein, saponins, flavonoid are the main pharmacodynamics compositions of the Radix Astragali.Radix Astragali total saponins has the protection blood vessel endothelium, improves the effects such as hemorheology, has protective effect aspect, amycin myocardium at hypoxic-ischemic cardiac muscle, viral infection and the isoproterenol injury of myocardium; Has protective effect aspect the arrhythmia that Radix Astragali total flavones causes at myocardial ischemia-reperfusion, acute myocardial infarction, viral myocarditis and barium chloride.This two large class active ingredient makes the Radix Astragali have significant curative effect aspect Cardiovarscular.
Disclose the preparation method of Radix Astragali injection in the 17 of the Traditional Chinese medicine historical preparation: the Radix Astragali decocts with water three times, collecting decoction, and filtrate is concentrated, with ethanol precipitation process secondary, containing amount of alcohol in the solution for the first time is 75%, is 85% for the second time, and each all cold preservation is placed, Recycled ethanol also is concentrated into every 1ml and is equivalent to crude drug 10g, be diluted to every 1ml with water for injection and be equivalent to crude drug 0.75～1g, cold preservation was placed 12 hours, filtered, filtrate is concentrated into every 1ml and is equivalent to crude drug 5～6g, let cool, regulate pH value to 7.5 with 20% sodium hydroxide solution, boil, the active carbon of adding 0.125%, boiled 5 minutes, and filtered while hot, inject water and make into 1000ml, filter, regulate pH value to 7.5 with 20% sodium hydroxide solution again, filter embedding, sterilization, and get final product.
Said method is traditional astragalus injection liquid preparing process, only astragaloside is tested the minimum 0.08mg/ml that is limited to of its content in the inspection item.In recent years, the research of more existing Technology improvement aspects.
Water extract-alcohol precipitation (normally preparing total polysaccharides and total saponins): write exactly in the background technology of CN200810045913.X, the preparation method of the conventional Radix Astragali is: the Radix Astragali decocts with water secondary, 3 hours for the first time, 2 hours for the second time, collecting decoction filtered, filtrate is concentrated into relative density approximately 1.26, adding ethanol makes it contain alcohol amount to be 70%, to stir evenly, leave standstill, get the supernatant Recycled ethanol, being concentrated into relative density is 1.36(38 ℃) clear paste.
(+)-Astragenol extract, Radix Astragali water extract, Radix Astragali water extract-alcohol precipitation extract, Radix Astragali semi-bionic extraction thing, Radix Astragali supercritical extract: CN200610000241.1 provide Chinese medicine preparation for the treatment of cardiovascular and cerebrovascular disease and preparation method thereof, disclose that Radix Astragali total saponins can be (+)-Astragenol extract, Radix Astragali water extract, Radix Astragali water extract-alcohol precipitation extract, Radix Astragali semi-bionic extraction thing, Radix Astragali supercritical extract in Radix Astragali total saponins liposome or the pro-liposome, but do not had the extracting method of clear and definite above-mentioned arbitrary extract.
Ben Yong light etc. discloses the cellulase solution and has extracted the total flavones (technical study of cellulose enzyme process extraction Radix Astragali total flavones, the time precious traditional Chinese medical science traditional Chinese medicines, 10 phases in 2009), take by weighing cellulase 8mg, with pH be after 4.5 HAc-NaAc buffer 10ml mixes with 1g Radix Astragali powder (mistake 50 mesh sieves) mix homogeneously, behind 30 ℃ of lower processing 1h, add 95% ethanol 20ml, filter at 70 ℃ of lower lixiviate 1h, with the washing with alcohol residue filter of 20ml volume fraction 85%, merging filtrate, Recycled ethanol, it is 85% ethanol that residue is dissolved in mass fraction, is settled to 25ml, and the accurate 1ml that draws is in the volumetric flask of 25ml, 30% ethanol standardize solution gets need testing solution.
CN200710012291.6 discloses a kind of method of preparing astragaloside iv by enzymic hydrolysis for astragalus saponin glycosyl, process the Radix Astragali or Radix Astragali total saponins with enzyme in the method, make the Radix Astragali saponin that contains the glycosyl more than three or three be converted into the astragaloside that contains two glycosyls, significantly improved the yield of astragaloside, but reduced the yield of other Radix Astragali saponin, this kind method only can prepare separately astragaloside.
CN99106225.6 discloses a kind of process for refining astragalus injection, its get the Radix Astragali by decoct, filter, concentrated, precipitate with ethanol 3 times then, concentration is 70%, 80%, 85%, behind each precipitate with ethanol 0 ℃ of cold preservation place a few hours, Recycled ethanol and concentrated, dilute with water for injection, cold preservation to 0 ℃-4 ℃, place 24 hours, filter, regulate pH value, boil and add active carbon, add 20% sodium hydroxide solution again with 20% sodium hydroxide solution, adjusting pH value, at last filtration, embedding, sterilization, and get final product.The method is used 3 precipitate with ethanol, although can remove more impurity, the also a large amount of loss of the content of effective ingredient.
CN03114789.5 discloses a kind of preparation method, it adopts the steps such as decocting boils, precipitate with ethanol, upper prop eluting to prepare formulation of astragalus root, the amount of astragaloside is not less than 0.032mg/ml in the preparation that the method obtains, glucoside content is lower, and the method adopts the technique of upper resin column behind the first precipitate with ethanol, may contain the pollutant such as degradation product of resin in the extract.
The extracting method that astragaloside is commonly used is, water extraction, and alkali treatment, organic solvent extraction, purification, preparation method and crude drug and preparation as CN200410007963.0 discloses a kind of astragaloside crude drug belong to modern Chinese traditional medicine field.The method is as follows: 1) extract: take the medical material that contains astragaloside as raw material, extract, filter, get extracting solution; 2) concentrated: the concentrated solution of 60 ℃ of lower relative densities 1.05～1.40 of extracting solution simmer down to; 3) alkali treatment: transferring pH is 8～14 or greater than 14; 4) separate astragaloside: the pH value to 5 of accent alkali treatment liquid～9, use organic solvent extraction, divide and get the organic solution layer; 5) purification: organic solvent layer is concentrated into dried, turns molten, adjust pH is 3～9, uses organic solvent extraction, flings to organic solvent, and white precipitate is separated out; 6) refining: centrifugal or filtration gained white precipitate, washing filters, and precipitation is dry, and recrystallization gets the astragaloside crude drug.
CN200710099116.5 discloses a kind of preparation method of Radix Astragali injection, and it adopts the steps such as decocting in water, upper prop eluting, precipitate with ethanol to prepare formulation of astragalus root.
CN201110218898.6 discloses the method for a kind of Radix Astragali ground, under ground portion comprehensive development and utilization, at first with ground or the under ground portion coarse powder of the Radix Astragali, then carrying out ultrasonic circulating with alcoholic solution extracts, alcohol extract passes through the absorption of ion exchange resin column or polyamide resin column, alcohol wash excessively after dealcoholysis, the concentrated Radix Astragali total flavones that obtains of pure washing liquid; Tail washings adsorbs through macroporous adsorptive resins, pure desorption, the concentrated Radix Astragali total saponins that obtains.
CN201210154465.3 is root 80% alcohol reflux of the Radix Astragali, and is concentrated, crosses the D101 resin, uses successively pure water, 15-25% ethanol, 60-95% ethanol elution, collects 60-95% ethanol elution part, reclaim under reduced pressure and get final product.
In addition, also there are some to pass through purify the separately research method of Radix Astragali total saponins or Radix Astragali total flavones of extracting process, the compositions of gained is the higher single classification of purity, can not improve simultaneously the content of Radix Astragali total saponins and Radix Astragali total flavones in traditional formulation of astragalus root technique, and the compositions that obtains or preparation do not had the effect that two large constituents are brought into play curative effect jointly.
Summary of the invention
The object of the invention is to provide that a kind of content is higher, the Radix Astragali injection of active ingredient reasonable mixture ratio, and this injection has better curative effect for the adjuvant therapy of cardiovascular disease.
The present invention also provides the preparation method of this injection.
A kind of Radix Astragali injection provided by the invention, contain two kinds of effective ingredient of astragaloside and calycosin glucoside, the described Radix Astragali injection of every ml contains astragaloside 0.08-0.8mg, contain calycosin glucoside 0.02-0.4mg, and astragaloside accounts for the 1%-10% of total solid, and the calycosin glucoside accounts for the 0.20%-5% of total solid;
Preferably, the described Radix Astragali injection of every ml contains astragaloside 0.09-0.6mg, contains calycosin glucoside 0.04-0.3mg, and astragaloside accounts for the 1.25%-7.5% of total solid, and the calycosin glucoside accounts for the 0.50%-3.75% of total solid.
Further preferred, the described Radix Astragali injection of every ml contains astragaloside 0.12-0.52mg, contains calycosin glucoside 0.05-0.25mg, and astragaloside accounts for the 1.5%-6.6% of total solid, and the calycosin glucoside accounts for the 0.60%-3.05% of total solid.
Injection provided by the invention can prepare by the following method:
1) Radix Astragali decocts with water 2-3 time, and collecting decoction filters, and is concentrated, adds ethanol and makes that to contain amount of alcohol be 70-75%, filter, and Recycled ethanol, thin up gets water extraction liquid, reclaims medicinal residues;
2) medicinal residues that reclaim alcohol reflux 2 times, merge extractive liquid,, Recycled ethanol, thin up gets alcohol extract;
3) merge water extraction liquid and alcohol extract, add ethanol and make and contain the alcohol amount and be 83%-87%, each all cold preservation is placed, and filters, and Recycled ethanol is to without the alcohol flavor, and thin up is regulated pH value, adds activated carbon adsorption, embedding, and sterilization, and get final product.
Preferably, described injection is prepared by following methods:
1) gets the Radix Astragali, decoct with water 2-3 time, add the water that 6-10 doubly measures at every turn, the each decoction 1.5-2 hour, collecting decoction filters, filtrate is concentrated into every 1ml and is equivalent to crude drug 1-2g, adds 95% ethanol and makes that to contain amount of alcohol be 70%-75%, and cold preservation was placed 12-36 hour, filter, Recycled ethanol also is concentrated into without the alcohol flavor, is diluted to every 1ml with water for injection and is equivalent to crude drug 2.5-4g, cold preservation was placed 12-36 hour, filter, get water extraction liquid, reclaim medicinal residues;
2) the 50%-95% alcohol reflux that the medicinal residues adding Radix Astragali volume 6-10 that reclaims doubly measures 2-3 time, each extraction time is 1.5-2 hour, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, be diluted to every 1ml with water for injection and be equivalent to crude drug 2.5-4g, cold preservation was placed 12-36 hour, filtered, and got alcohol extract;
3) merge water extraction liquid and alcohol extract, add 95% ethanol and make and contain the alcohol amount and be 83%-87%, cold preservation was placed 12-36 hour, filter, Recycled ethanol is diluted to every 1ml with water for injection and is equivalent to crude drug 5-6g to without the alcohol flavor, let cool, regulate pH value to 7.5-8.5 with 20% sodium hydroxide solution, boil, the active carbon that adds the 1-2% of medical material weight boils, and filters while hot, regulates pH value to 7.0-8.0 with 20% sodium hydroxide solution again, filter, embedding, sterilization, and get final product.
Preferably, described injection is prepared by following methods:
1) gets the Radix Astragali, decoct with water 2-3 time, add the water that 6-10 doubly measures at every turn, the each decoction 1.5-2 hour, collecting decoction filters, filtrate is concentrated into every 1ml and is equivalent to crude drug 1.34-1.44g, adds 95% ethanol and makes that to contain amount of alcohol be 73-75%, and cold preservation was placed 20-36 hour, filter, Recycled ethanol also is concentrated into without the alcohol flavor, is diluted to every 1ml with water for injection and is equivalent to crude drug 2.60-2.80g, cold preservation was placed 20-36 hour, filter, get water extraction liquid, reclaim medicinal residues;
2) the 60-80% alcohol reflux that the medicinal residues adding Radix Astragali volume 6-10 that reclaims doubly measures 2 times, each extraction time is 1.5-2 hour, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, be diluted to every 1ml with water for injection and be equivalent to crude drug 2.60-2.80g, cold preservation was placed 20-36 hour, filtered, and got alcohol extract;
3) merge water extraction liquid and alcohol extract, add 95% ethanol and make and contain the alcohol amount and be 84-87%, cold preservation was placed 20-36 hour, filter, Recycled ethanol is diluted to every 1ml with water for injection and is equivalent to crude drug 5.30-5.70g to without the alcohol flavor, let cool, regulate pH value to 7.6-8.4 with 20% sodium hydroxide solution, boil, the active carbon that adds the 1.5-2.0% of medical material weight boils, and filters while hot, regulates pH value to 7.3-8.0 with 20% sodium hydroxide solution again, filter, embedding, sterilization, and get final product.
Further preferred, described injection is prepared by following methods:
1) gets the Radix Astragali, decoct with water 2-3 time, add the water that 6-10 doubly measures at every turn, the each decoction 1.5-2 hour, collecting decoction filters, filtrate is concentrated into every 1ml and is equivalent to crude drug 1.36-1.41g, adds 95% ethanol and makes that to contain amount of alcohol be 74-75%, and cold preservation was placed 24-30 hour, filter, Recycled ethanol also is concentrated into without the alcohol flavor, is diluted to every 1ml with water for injection and is equivalent to crude drug 2.68-2.70g, cold preservation was placed 24-30 hour, filter, get water extraction liquid, reclaim medicinal residues;
2) the 65-75% alcohol reflux that the medicinal residues adding Radix Astragali volume 6-10 that reclaims doubly measures 2 times, each extraction time is 1.5-2 hour, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, be diluted to every 1ml with water for injection and be equivalent to crude drug 2.65-2.75g, cold preservation was placed 24-30 hour, filtered, and got alcohol extract;
3) merge water extraction liquid and alcohol extract, add 95% ethanol and make and contain the alcohol amount and be 85-87%, cold preservation was placed 24-30 hour, filter, Recycled ethanol is diluted to every 1ml with water for injection and is equivalent to crude drug 5.45-5.65g to without the alcohol flavor, let cool, regulate pH value to 7.8-8.2 with 20% sodium hydroxide solution, boil, the active carbon that adds the 1.5-2.0% of medical material weight boils, and filters while hot, regulates pH value to 7.5-7.8 with 20% sodium hydroxide solution again, filter, embedding, sterilization, and get final product.
The present invention also provides the preparation method of above-mentioned injection, may further comprise the steps:
1) Radix Astragali decocts with water 2-3 time, and collecting decoction filters, and is concentrated, adds ethanol and makes that to contain amount of alcohol be 70-75%, filter, and Recycled ethanol, thin up gets water extraction liquid, reclaims medicinal residues;
2) medicinal residues that reclaim alcohol reflux 2 times, merge extractive liquid,, Recycled ethanol, thin up gets alcohol extract;
3) merge water extraction liquid and alcohol extract, add ethanol and make and contain the alcohol amount and be 83%-87%, each all cold preservation is placed, and filters, and Recycled ethanol is to without the alcohol flavor, and thin up is regulated pH value, adds activated carbon adsorption, adds water to amount of preparation, filter, and embedding, sterilization, and get final product.
The present invention also provides the application of above-mentioned Radix Astragali injection in preparation treatment myocarditis, myocardial ischemia, heart failure, myocardial infarction, ARR medicine.
Radix Astragali injection provided by the invention has the following advantages:
1, preparation method:
Existing method is used separately water extraction or alcohol extraction, can not improve simultaneously the content of astragaloside and calycosin glucoside.
1) method of using water extraction to combine with alcohol extraction in the extracting method of the present invention, by adjusting precipitate with ethanol step, precipitate with ethanol parameter and to the adjusting of pH value, can extract simultaneously the higher astragaloside of content and calycosin glucoside, compared with prior art, the content of calycosin glucoside improves 2-50 doubly;
2) compared with prior art, do not use any organic reagent except ethanol, Product quality and safety.
3) extracting method is simple, and is easy to operate.
2, injection provided by the invention all has preferably auxiliary therapeutic action aspect treatment myocarditis, myocardial ischemia, heart failure, myocardial infarction, the arrhythmia, and effect is better than prior art.
3, injection active constituent content provided by the invention is high, simultaneously its effective ingredient is accounted for the control of the amount of total solid, so that proportioning is more reasonable, and good effect, steady quality.
The specific embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
If no special instructions, concentration of alcohol of the present invention is volume ratio, is that the volume ratio of 95% ethanol and water is 70:25 with the preparation of 95% ethanol such as 70% ethanol.
Embodiment 1: Radix Astragali injection
1, gets Radix Astragali 1000g, decoct with water 2 times, add respectively the water of 10 times of amounts of astragalus weight, 8 times of amounts, the each decoction 2 hours merges decoction liquor, filters, filtrate is concentrated into the every 1ml of 745ml(and is equivalent to crude drug 1.34g), add 95% ethanol and make that to contain amount of alcohol be 73%, cold preservation was placed 20 hours, filter, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 385ml(and is equivalent to crude drug 2.60g), cold preservation was placed 20 hours, filter, get water extraction liquid, reclaim medicinal residues;
2, the medicinal residues that reclaim alcohol reflux 2 times, each 60% ethanol that adds 8 times of amounts of Radix Astragali volume, extraction time is each 1.5 hours, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 380ml(and is equivalent to crude drug 2.63g), cold preservation was placed 20 hours, filter, get alcohol extract;
3, merge water extraction liquid and alcohol extract, add 95% ethanol and make that to contain alcohol amount be 84%, cold preservation was placed 20 hours, filter, Recycled ethanol is diluted to the every 1ml of 188ml(with water for injection and is equivalent to crude drug 5.32g to without the alcohol flavor), let cool, regulate pH value to 7.6 with 20% sodium hydroxide solution, boil, add 20g(account for medical material weight 2.0%) active carbon boil, filter while hot, inject water and make into 500ml, filter, regulate pH value to 8.0 with 20% sodium hydroxide solution again, filter, embedding, sterilization namely gets Radix Astragali injection.
Embodiment 2: Radix Astragali injection
1, gets Radix Astragali 1000g, decoct with water 2 times, the decocting that adds for the first time 8 times of amounts of astragalus weight boiled 2 hours, the decocting that adds for the second time 6 times of amounts boiled 1.5 hours, merge decoction liquor, filter, filtrate is concentrated into the every 1ml of 675ml(and is equivalent to crude drug 1.48g), add 95% ethanol and make that to contain amount of alcohol be 70%, cold preservation was placed 18 hours, filter, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 392ml(and is equivalent to crude drug 2.55g), cold preservation was placed 18 hours, filter, get water extraction liquid, reclaim medicinal residues;
2, the medicinal residues that reclaim alcohol reflux 2 times, each 50% ethanol that adds 8 times of amounts of Radix Astragali volume, 6 times of amounts, extraction time was respectively 2 hours, 1.5 hours, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, adding water for injection is diluted to the every 1ml of 387ml(and is equivalent to crude drug 2.58g), cold preservation was placed 18 hours, got alcohol extract;
3, merge water extraction liquid and alcohol extract, add 95% ethanol and make that to contain alcohol amount be 83%, cold preservation was placed 18 hours, filter, Recycled ethanol is diluted to the every 1ml of 194ml(with water for injection and is equivalent to crude drug 5.15g to without the alcohol flavor), let cool, regulate pH value to 8.5 with 20% sodium hydroxide solution, boil, add 10g(account for medical material weight 1%) active carbon boil, filter while hot, inject water and make into 500ml, filter, regulate pH value to 8.0 with 20% sodium hydroxide solution again, filter, embedding, sterilization namely gets Radix Astragali injection.
Embodiment 3: Radix Astragali injection
1, gets Radix Astragali 1000g, decoct with water 3 times, the water that adds respectively 10 times of amounts of astragalus weight, 8 times of amounts, 8 times of amounts, the each decoction 1.5 hours, merge decoction liquor, filter, filtrate is concentrated into the every 1ml of 688ml(and is equivalent to crude drug 1.45g), add 95% ethanol and make that to contain amount of alcohol be 72%, cold preservation was placed 12 hours, filter, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 396ml(and is equivalent to crude drug 2.53g), cold preservation was placed 12 hours, filter, get water extraction liquid, reclaim medicinal residues;
2, the medicinal residues that reclaim alcohol reflux 2 times, each 10 times of amounts of Radix Astragali volume, 95% ethanol of 8 times of amounts of adding, extraction time is 1.5 hours, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 377ml(and is equivalent to crude drug 2.65g), cold preservation was placed 12 hours, filter, get alcohol extract;
3, merge water extraction liquid and alcohol extract, add 95% ethanol and make that to contain alcohol amount be 82%, cold preservation was placed 12 hours, filter, Recycled ethanol is diluted to the every 1ml of 199ml(with water for injection and is equivalent to crude drug 5.03g to without the alcohol flavor), let cool, regulate pH value to 7.5 with 20% sodium hydroxide solution, boil, add 10g(account for medical material weight 1%) active carbon boil, filter while hot, inject water and make into 500ml, filter, regulate pH value to 7.0 with 20% sodium hydroxide solution again, filter, embedding, sterilization namely gets Radix Astragali injection.
Embodiment 4: Radix Astragali injection
1, gets Radix Astragali 1000g, decoct with water 3 times, the water that adds respectively 10 times of amounts of astragalus weight, 8 times of amounts, 6 times of amounts, the each decoction 1.5 hours, merge decoction liquor, filter, filtrate is concentrated into the every 1ml of 693ml(and is equivalent to crude drug 1.44g), add 95% ethanol and make that to contain amount of alcohol be 75%, cold preservation was placed 36 hours, filter, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 362ml(and is equivalent to crude drug 2.76g), cold preservation was placed 36 hours, filter, get water extraction liquid, reclaim medicinal residues;
2, the medicinal residues that reclaim alcohol reflux 2 times, 80% ethanol that adds respectively 10 times of amounts of Radix Astragali volume, 8 times of amounts, extraction time is 2 hours, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 357ml(and is equivalent to crude drug 2.80g), cold preservation was placed 36 hours, filter, get alcohol extract;
3, merge water extraction liquid and alcohol extract, add 95% ethanol and make that to contain alcohol amount be 87%, cold preservation was placed 36 hours, filter, Recycled ethanol is diluted to the every 1ml of 178ml(with water for injection and is equivalent to crude drug 5.62g to without the alcohol flavor), let cool, regulate pH value to 8.4 with 20% sodium hydroxide solution, boil, add 15g(account for medical material weight 1.5%) active carbon boil, filter while hot, inject water and make into 500ml, filter, regulate pH value to 7.3 with 20% sodium hydroxide solution again, filter, embedding, sterilization, and get final product.
Embodiment 5: Radix Astragali injection
1, gets Radix Astragali 1000g, decoct with water 2 times, the water that adds respectively 8 times of amounts of astragalus weight, 6 times of amounts, decocted respectively 2 hours, 1.5 hours, merge decoction liquor, filter, filtrate is concentrated into the every 1ml of 733ml(and is equivalent to crude drug 1.36g), add 95% ethanol and make that to contain amount of alcohol be 75%, cold preservation was placed 24 hours, filter, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 373ml(and is equivalent to crude drug 2.68g), cold preservation was placed 24 hours, filter, get water extraction liquid, reclaim medicinal residues;
2, the medicinal residues that reclaim alcohol reflux 2 times, 65% ethanol that adds respectively 8 times of amounts of Radix Astragali volume, 6 times of amounts, extraction time is 1.5 hours, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 377ml(and is equivalent to crude drug 2.65g), cold preservation was placed 24 hours, filter, get alcohol extract;
3, merge water extraction liquid and alcohol extract, add 95% ethanol and make that to contain alcohol amount be 85%, cold preservation was placed 24 hours, filter, Recycled ethanol is diluted to the every 1ml of 177ml(with water for injection and is equivalent to crude drug 5.65g to without the alcohol flavor), let cool, regulate pH value to 8.2 with 20% sodium hydroxide solution, boil, add 15g(account for medical material weight 1.5%) active carbon boil, filter while hot, inject water and make into 500ml, filter, regulate pH value to 7.8 with 20% sodium hydroxide solution again, filter, embedding, sterilization namely gets Radix Astragali injection.
Embodiment 6: Radix Astragali injection
1, gets Radix Astragali 1000g, decoct with water 3 times, the water that adds respectively 8 times of amounts of astragalus weight, 8 times of amounts, 6 times of amounts, the each decoction 1.5 hours, merge decoction liquor, filter, filtrate is concentrated into the every 1ml of 718ml(and is equivalent to crude drug 1.39g), add 95% ethanol and make that to contain amount of alcohol be 74%, cold preservation was placed 28 hours, filter, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 370ml(and is equivalent to crude drug 2.70g), cold preservation was placed 28 hours, filter, get water extraction liquid, reclaim medicinal residues;
2, the medicinal residues that reclaim alcohol reflux 2 times, 75% ethanol that adds respectively 10 times of amounts of Radix Astragali volume, 8 times of amounts, extraction time is 2 hours, 1.5 hours, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 364ml(and is equivalent to crude drug 2.75g), cold preservation was placed 28 hours, filter, get alcohol extract;
3, merge water extraction liquid and alcohol extract, add 95% ethanol and make that to contain alcohol amount be 87%, cold preservation was placed 28 hours, filter, Recycled ethanol is diluted to the every 1ml of 181ml(with water for injection and is equivalent to crude drug 5.52g to without the alcohol flavor), let cool, regulate pH value to 7.8 with 20% sodium hydroxide solution, boil, add 20g(account for medical material weight 2%) active carbon boil, filter while hot, inject water and make into 500ml, filter, regulate pH value to 7.6 with 20% sodium hydroxide solution again, filter, embedding, sterilization namely gets Radix Astragali injection.
Embodiment 7: Radix Astragali injection
1, gets Radix Astragali 1000g, decoct with water 2 times, add the water of 10 times of amounts of astragalus weight at every turn, the each decoction 1.5 hours merges decoction liquor, filters, filtrate is concentrated into the every 1ml of 709ml(and is equivalent to crude drug 1.41g), add 95% ethanol and make that to contain amount of alcohol be 74%, cold preservation was placed 30 hours, filter, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 377ml(and is equivalent to crude drug 2.65g), cold preservation was placed 30 hours, filter, get water extraction liquid, reclaim medicinal residues;
2, the medicinal residues that reclaim alcohol reflux 2 times, each 70% ethanol that adds 8 times of amounts of Radix Astragali volume, extraction time is 2 hours, 1.5 hours, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, and adding water for injection is diluted to the every 1ml of 370ml(and is equivalent to crude drug 2.70g), cold preservation was placed 30 hours, filter, get alcohol extract;
3, merge water extraction liquid and alcohol extract, add 95% ethanol and make that to contain alcohol amount be 86%, cold preservation was placed 30 hours, filter, Recycled ethanol is diluted to the every 1ml of 183ml(with water for injection and is equivalent to crude drug 5.45g to without the alcohol flavor), let cool, regulate pH value to 8.0 with 20% sodium hydroxide solution, boil, add 15g(account for medical material weight 1.5%) active carbon boil, filter while hot, inject water and make into 500ml, filter, regulate pH value to 7.5 with 20% sodium hydroxide solution again, filter, embedding, sterilization namely gets Radix Astragali injection.
Comparative Examples 1: Radix Astragali injection
With reference to the preparation method of Radix Astragali injection in the 17 of the Traditional Chinese medicine historical preparation, concrete preparation method is:
The Radix Astragali decocts with water three times, collecting decoction, and filtrate is concentrated, with ethanol precipitation process secondary, containing amount of alcohol in the solution for the first time is 75%, is 85% for the second time, each all cold preservation is placed, and Recycled ethanol also is concentrated into every 1ml and is equivalent to crude drug 10g, is diluted to every 1ml with water for injection and is equivalent to crude drug 0.75g, cold preservation was placed 12 hours, filtered, and filtrate is concentrated into every 1ml and is equivalent to crude drug 6g, let cool, regulate pH value to 7.5 with 20% sodium hydroxide solution, boil, the active carbon of adding 0.125%, boiled 5 minutes, and filtered while hot, inject water and make into 1000ml, filter, regulate pH value to 7.5 with 20% sodium hydroxide solution again, filter embedding, sterilization, and get final product.
Comparative Examples 2: Radix Astragali injection
With reference to the embodiment 1 of CN99106225.6, concrete preparation method is:
1, get Radix Astragali 2000g, add respectively 10 times of amounts, 8 times of water gagings decoct 2 times, each 1.5 hours, merging filtrate filtered through filter, and the filtrate normal heating is concentrated into every 1ml and is equivalent to crude drug 1g;
2, use ethanol precipitation process 3 times, in filtrate, add for the first time content and be 3 liters of 70% ethanol, behind the precipitate with ethanol, 0 ℃ of cold preservation was placed 6 hours, added content for the second time again and be 2 liters of 80% ethanol, behind the precipitate with ethanol, 0 ℃ of placement of cold preservation 6 hours, add for the third time content again and be 3 liters of 85% ethanol, behind the precipitate with ethanol, 0 ℃ of cold preservation was placed 6 hours;
3, Recycled ethanol is concentrated into the 10g that 1ml is equivalent to crude drug, be diluted to the 0.8g that every 1ml is equivalent to crude drug with water for injection, cold preservation to 0 ℃, placed 24 hours, filter, filtrate is concentrated into the 5.5g that every 1ml is equivalent to crude drug, cooling, regulate pH value to 7.3 with 20% sodium hydroxide solution, the active carbon that boils adding 0.125% stirs, and boils 5 minutes, is cooled to 50 ℃ and uses the filter filtered while hot, inject water and make into 1000ml, add again 20% sodium hydroxide solution 2mol/L, regulate pH value to 7.5, filter at last, embedding, sterilization, quality inspection, packing forms.
Comparative Examples 3: Radix Astragali injection
With reference to the embodiment 1 of CN200710099116.5, concrete preparation method is:
1, Radix Astragali section adds the water of 8 times of amounts of crude drug, and 60 ℃ of warm macerating 30 minutes boiled 1.5 hours, leached, and added the water of 6 times of amounts of crude drug, boiled 1 hour;
2, merging filtrate, cooling was left standstill 1 hour, filtered, and was cooled to below 30 ℃; Upper resin column soaked 30 minutes, crossed post absorption with the flow velocity of 18 liter/mins of clocks, rushed post with the purified water of 3 times of amounts of resin, then 30% ethanol with 1 times of amount of resin rushes post, rush post with the purified water of 1 times of amount of resin again, 70% ethanol with 4 times of amounts of resin soaked 30 minutes at last, with 15 liter/mins of clock flow velocity eluting;
Collect eluent, filter, Recycled ethanol is nothing alcohol flavor extremely, and is concentrated into relative density 1.16 ± 0.02 (80 ℃ ± 2 survey).Add high alcohol and make and contain alcohol amount and reach 85%, room temperature left standstill 12 hours, 0.45 μ m membrane filtration, and Recycled ethanol is to without the alcohol flavor; Inject water to every 1ml and contain crude drug in whole 2g, stirring and dissolving, adjust pH to 3.2, fill, 115 ℃ of autoclavings 40 minutes, be refrigerated to icing, 0 ℃ of cold preservation 7 days;
3, with cold preservation liquid through 0.45 μ m filtering with microporous membrane, transfer pH9.0 with sodium hydroxide, add 0.1% active carbon and boiled 15 minutes, treat to filter below the drop in temperature to 50 ℃, through 115 ℃ of sterilizations 40 minutes.Be refrigerated to the rear timely negative catalysis of taking out of freezing, in shady and cool dry locating or room temperature placement two weeks;
4, filter with 200 order silks, again through 0.2 μ m filtering with microporous membrane, after 6000 molecular weight ultrafilter ultrafiltration, get ultrafiltrate.The water for injection after itself and the ultrafiltration below 40 ℃ is merged, with 10%NaOH adjust pH 9.5, the water for injection of adding again after the ultrafiltration contains crude drug in whole 2g to every 1ml again.Treat that medicinal liquid is cooled to below 30 ℃ through 0.2 μ m microporous filter membrane, skeleton symbol germ tight filter fine straining, fill sterilization and get final product.
Experimental example 1: content detection
The Radix Astragali injection that embodiment 1-7 and Comparative Examples 1-3 are provided carries out content detection, mainly detects the content of astragaloside and calycosin glucoside.
1, detection method of content is as follows:
1) astragaloside
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filler; Take methanol-water (70:30) as mobile phase; Evaporative light scattering detector.Number of theoretical plate should be not less than 2000 in the astragaloside peak.
It is an amount of that the preparation precision of reference substance solution takes by weighing the astragaloside reference substance, adds methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.
The preparation of need testing solution is got this product as need testing solution.
Accurate reference substance solution 4 μ l, 8 μ l, the 16 μ l of drawing of algoscopy, need testing solution 5～10 μ l, the injection liquid chromatography is measured, and calculates with external standard line-of-sight course logarithmic equation, and get final product.
2) assay of calycosin glucoside: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 D).
Chromatographic condition and system suitability take acetonitrile as mobile phase A, take water as Mobile phase B, carry out gradient elution by table 1 take octadecylsilane chemically bonded silica as filler; Flow velocity is per minute 1.0ml; The detection wavelength is 260nm.Column temperature is 30 ℃, and number of theoretical plate calculates by calycosin glucoside peak should be not less than 3000.
Table 1: gradient elution
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～40 | 3→30 | 97→70 |
| 40～65 | 30→85 | 70→15 |
| 65～75 | 85 | 15 |
| 75～80 | 85→3 | 15→97 |
It is an amount of, accurately weighed that calycosin glucoside reference substance is got in the preparation of reference substance solution, adds 20% acetonitrile and make the solution that every 1ml contains 0.1mg, and get final product.
The accurate this product 2ml that draws of the preparation of need testing solution puts in the 20ml measuring bottle, and thin up shakes up to scale, filters with 0.45 μ m microporous filter membrane, gets subsequent filtrate, and get final product.
Algoscopy is accurate reference substance solution and each 20 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product.
2, astragaloside and calycosin glucoside account for the computational methods of total solids content among total solids content and each embodiment:
1) amount of total solid: precision measures Radix Astragali injection 50ml, puts in the evaporating dish that is dried to constant weight evaporate to dryness in the water-bath, 105 ℃ of dryings 3 hours, in the dislocation exsiccator, cooled off 30 minutes, rapid accurately weighed weight is calculated the amount (g/ml) that namely gets total solid;
2) astragaloside accounts for the amount (%) of total solid=(Astragaloside content/total solid) * 100%
3) the calycosin glucoside accounts for the amount (%) of total solid=(calycosin glucoside content/total solid) * 100%
3, testing result: see Table 2
Table 2: the content of Comparative Examples and the embodiment of the invention relatively
Table 2 result shows: compare with Comparative Examples, the content of calycosin glucoside is obviously higher in the Radix Astragali injection provided by the invention.
Experimental example 2: Radix Astragali injection is to the effect of myocardial ischemia
1, laboratory animal: the Wistar rat, body weight 250g-300g, male.
2, experiment grouping:
120 rats are divided into 12 groups at random: sham operated rats, model control group, embodiment 1-7 group, Comparative Examples 1-3 group, 10 every group, dosage:
Sham operated rats: normal saline 1ml/100g body weight;
Model control group: normal saline 1ml/100g body weight;
Embodiment 1-7 group and Comparative Examples 1-3 group: test sample 1ml/100g body weight (the 1ml sample is equivalent to contain crude drug 2g).
3, experimental technique:
1) pentobarbital (80mg/kg) intraperitoneal injection of anesthesia is measured normal II and is led electrocardiogram, cuts breastbone, takes out heart, with 6-0 silk thread 2mm place ligation arteria coronaria left anterior descending branch under left auricle, then heart is put back to the thoracic cavity, extracts air in the thoracic cavity out, sews up.
2) behind the ligation 10min, according to experiment grouping administration, and the II that records in 2 hours is led electrocardiogram.Animal sent back in the cage raise, abdominal aortic blood after 24 hours, low temperature (4 ℃) preparation serum is measured AST, LDH, CK-MB Biochemical Indices In Serum.
4, statistical method: adopt the SPSS11.0 statistical package to carry out statistical analysis.
5, experimental result:
Table 3: embodiment and comparative example are on the impact of myocardial ischemia in rats
Annotate: compare with sham operated rats,
※P＜0.05,
※ ※P＜0.01; Compare with model control group,
*P＜0.05,
*P＜0.01; Compare with the Comparative Examples group respectively,
#P＜0.05.
Table 3 result shows:
Compare with sham operated rats: model group ST section is moved with the T ripple on significantly and is significantly raise (p＜0.01), and serum AST, LDH, CK-MB value significantly increase (p＜0.01), illustrate that modeling successfully;
Behind the rat vein input medicine, compare with model group, move with T ripple rising amplitude and significantly reduce (p＜0.01) on ST section of each group of embodiment 1-7, serum AST, LDH, CK-MB value also significantly raise (p＜0.01) Comparative Examples each organize notable difference (p＜0.05) also arranged;
Respectively organize with Comparative Examples respectively and compare, move on the ST section of embodiment 1-7 group and T ripple rising amplitude reduction obvious (p＜0.05), serum AST, LDH, CK-MB value be obviously rising (p＜0.05) also;
Simultaneously, effect of each group of 1 group, 4 groups of embodiment, 5-7 slightly is better than embodiment 2,3 effect, and the effect of embodiment 5-7 group slightly is better than 1 group of embodiment, 4 groups effect.
Experimental result shows, Radix Astragali injection provided by the invention has obvious curative effect to myocardial ischemia, and effect is better than prior art.
Experimental example 3: the effect for the treatment of viral myocarditis
1, laboratory animal: Balb/c mice, body weight 16-20g.
2, experiment grouping: 220 mices, be divided at random 12 groups, wherein the blank group is 10,10 of virus control groups, embodiment 1-7 respectively organizes 20, and Comparative Examples 1-3 respectively organizes 20.
3, experimental technique:
Blank group: according to 1ml/100g gavage distilled water;
Virus control group: every intraperitoneal inoculation 0.1CVB
3Virus liquid (TCID
50=10
-7.5, 10
5Doubly dilution), according to 1ml/100g gavage distilled water;
Experimental example 1-7 group and Comparative Examples 1-3 group: every intraperitoneal inoculation 0.1CVB
3Virus liquid (TCID
50=10
-7.5, 10
5Doubly dilution), by 1ml/100g gastric infusion (1ml is equivalent to contain crude drug 2g), successive administration 7 days was observed to the 15th day.
4, observation index: the mental status of animal, diet, hair color and death condition during the observed and recorded administration.
5, statistical method: adopt the SPSS11.0 statistical package to carry out statistical analysis.
6, result of the test: see Table 4
Table 4: anti-CVB
3The survival number of virus and survival rate are relatively
| Number of animals (only) | Survival number (only) | Survival rate (%) | |
| The blank group | 10 | 10 | 100 |
| The virus control group | 10 | 2 | 20 ※※ |
| 1 group of embodiment | 20 | 17 | 85 **# |
| 2 groups of embodiment | 20 | 16 | 80 **# |
| 3 groups of embodiment | 20 | 15 | 75 **# |
| 4 groups of embodiment | 20 | 17 | 85 **# |
| 5 groups of embodiment | 20 | 18 | 90 **# |
| 6 groups of embodiment | 20 | 18 | 90 **# |
| 7 groups of embodiment | 20 | 18 | 90 **# |
| 1 group of Comparative Examples | 20 | 13 | 65 * |
| 2 groups of Comparative Examples | 20 | 14 | 70 * |
| 3 groups of Comparative Examples | 20 | 13 | 65 * |
Annotate: compare with blank,
※ ※P＜0.01; Compare with the virus control group,
*P＜0.05,
*P＜0.01; Compare with the Comparative Examples group,
#P＜0.05.
Table 4 result shows:
Infect CVB
3After the virus, each was organized the mice major part and showed obvious infection symptoms after 3 day.
Infect in viral rear 15 days, compare with the blank group, virus control group mice dies from serious dyspnea in succession, only survives 2, and survival rate significantly reduces (p＜0.01).
Compare with the virus control group, each group of embodiment 1-7 and Comparative Examples 1-3 respectively organize mice also incidence generation in succession, and it is lighter that embodiment 1-7 respectively organizes infection symptoms, survival rate, life span all be significantly increased (p＜0.01); It is lighter that Comparative Examples 1-3 respectively organizes infection symptoms, survival rate, life span all be significantly improved (p＜0.05);
Compare with each group of Comparative Examples respectively, survival rate, the life span of each group of embodiment 1-7 all are higher than the Comparative Examples group, and significant difference (p＜0.05) occurs;
Simultaneously, effect of each group of 1 group, 4 groups of embodiment, 5-7 slightly is better than embodiment 2,3 effect, and the effect of embodiment 5-7 group slightly is better than 1 group of embodiment, 4 groups effect.
Experimental result shows, injection of the present invention is to infecting CVB
3The mice of virus has certain therapeutical effect, and effect is better than prior art.
Although, above used general explanation, the specific embodiment and test, the present invention is described in detail, on basis of the present invention, can make some modifications or improvements it, and this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (9)
1. Radix Astragali injection, it is characterized in that, this injection contains astragaloside and two kinds of effective ingredient of calycosin glucoside, every ml Radix Astragali injection contains astragaloside 0.08-0.8mg, contain calycosin glucoside 0.02-0.4mg, and astragaloside accounts for the 1%-10% of total solid, and the calycosin glucoside accounts for the 0.20%-5% of total solid.
2. injection according to claim 1, it is characterized in that, in the described Radix Astragali injection, every ml Radix Astragali injection contains astragaloside 0.09-0.6mg, contain calycosin glucoside 0.04-0.3mg, and astragaloside accounts for the 1.25%-7.5% of total solid, and the calycosin glucoside accounts for the 0.50%-3.75% of total solid.
3. injection according to claim 1, it is characterized in that, the described Radix Astragali injection of every ml contains astragaloside 0.12-0.52mg, contain calycosin glucoside 0.05-0.25mg, and astragaloside accounts for the 1.5%-6.6% of total solid, and the calycosin glucoside accounts for the 0.60%-3.05% of total solid.
4. each described injection is characterized in that according to claim 1-3, and this injection is prepared by following methods:
1) Radix Astragali decocts with water 2-3 time, and collecting decoction filters, and is concentrated, adds ethanol and makes that to contain amount of alcohol be 70-75%, filter, and Recycled ethanol, thin up gets water extraction liquid, reclaims medicinal residues;
2) medicinal residues that reclaim alcohol reflux 2 times, merge extractive liquid,, Recycled ethanol, thin up gets alcohol extract;
3) merge water extraction liquid and alcohol extract, add ethanol and make and contain the alcohol amount and be 83%-87%, each all cold preservation is placed, and filters, and Recycled ethanol is to without the alcohol flavor, and thin up is regulated pH value, adds activated carbon adsorption, adds water to amount of preparation, filter, and embedding, sterilization, and get final product.
5. injection according to claim 4 is characterized in that, this injection is prepared by following methods:
1) gets the Radix Astragali, decoct with water 2-3 time, add the water that 6-10 doubly measures at every turn, the each decoction 1.5-2 hour, collecting decoction filters, filtrate is concentrated into every 1ml and is equivalent to crude drug 1-2g, adds 95% ethanol and makes that to contain amount of alcohol be 70-75%, and cold preservation was placed 12-36 hour, filter, Recycled ethanol also is concentrated into without the alcohol flavor, is diluted to every 1ml with water for injection and is equivalent to crude drug 2.5-4g, cold preservation was placed 12-36 hour, filter, get water extraction liquid, reclaim medicinal residues;
2) 6-10 that the medicinal residues that reclaim add the Radix Astragali doubly measures the 50%-95% alcohol reflux 2-3 time, each extraction time is 1.5-2 hour, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, be diluted to every 1ml with water for injection and be equivalent to crude drug 2.5-4g, cold preservation was placed 12-36 hour, filtered, and got alcohol extract;
3) merge water extraction liquid and alcohol extract, add ethanol and make and contain the alcohol amount and be 83%-87%, cold preservation was placed 12-36 hour, filter, Recycled ethanol is diluted to every 1ml with water for injection and is equivalent to crude drug 5-6g to without the alcohol flavor, let cool, regulate pH value to 7.5-8.5 with 20% sodium hydroxide solution, boil, the active carbon that adds the 1-2% of medical material weight boils, and filters while hot, injects water and makes into 1000ml, filter, regulate pH value to 7.0-8.0 with 20% sodium hydroxide solution again, filter, embedding, sterilization, and get final product.
6. injection according to claim 4 is characterized in that, this injection is prepared by following methods:
1) gets the Radix Astragali, decoct with water 2-3 time, add the water that 6-10 doubly measures at every turn, the each decoction 1.5-2 hour, collecting decoction filters, filtrate is concentrated into every 1ml and is equivalent to crude drug 1.34-1.44g, adds 95% ethanol and makes that to contain amount of alcohol be 73-75%, and cold preservation was placed 20-36 hour, filter, Recycled ethanol also is concentrated into without the alcohol flavor, is diluted to every 1ml with water for injection and is equivalent to crude drug 2.60-2.80g, cold preservation was placed 20-36 hour, filter, get water extraction liquid, reclaim medicinal residues;
2) the 60-80% alcohol reflux that the medicinal residues adding Radix Astragali volume 6-10 that reclaims doubly measures 2 times, each extraction time is 1.5-2 hour, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, be diluted to every 1ml with water for injection and be equivalent to crude drug 2.60-2.80g, cold preservation was placed 20-36 hour, filtered, and got alcohol extract;
3) merge water extraction liquid and alcohol extract, add 95% ethanol and make and contain the alcohol amount and be 84-87%, cold preservation was placed 20-36 hour, filter, Recycled ethanol is diluted to every 1ml with water for injection and is equivalent to crude drug 5.30-5.70g to without the alcohol flavor, let cool, regulate pH value to 7.6-8.4 with 20% sodium hydroxide solution, boil, the active carbon that adds the 1.5-2.0% of medical material weight boils, and filters while hot, regulates pH value to 7.3-8.0 with 20% sodium hydroxide solution again, filter, embedding, sterilization, and get final product.
7. injection according to claim 4 is characterized in that, described injection is prepared by following methods:
1) gets the Radix Astragali, decoct with water 2-3 time, add the water that 6-10 doubly measures at every turn, the each decoction 1.5-2 hour, collecting decoction filters, filtrate is concentrated into every 1ml and is equivalent to crude drug 1.36-1.41g, adds 95% ethanol and makes that to contain amount of alcohol be 74-75%, and cold preservation was placed 24-30 hour, filter, Recycled ethanol also is concentrated into without the alcohol flavor, is diluted to every 1ml with water for injection and is equivalent to crude drug 2.68-2.70g, cold preservation was placed 24-30 hour, filter, get water extraction liquid, reclaim medicinal residues;
2) the 65-75% alcohol reflux that the medicinal residues adding Radix Astragali volume 6-10 that reclaims doubly measures 2 times, each extraction time is 1.5-2 hour, merge extractive liquid,, Recycled ethanol also is concentrated into without the alcohol flavor, be diluted to every 1ml with water for injection and be equivalent to crude drug 2.65-2.75g, cold preservation was placed 24-30 hour, filtered, and got alcohol extract;
3) merge water extraction liquid and alcohol extract, add 95% ethanol and make and contain the alcohol amount and be 85-87%, cold preservation was placed 24-30 hour, filter, Recycled ethanol is diluted to every 1ml with water for injection and is equivalent to crude drug 5.45-5.65g to without the alcohol flavor, let cool, regulate pH value to 7.8-8.2 with 20% sodium hydroxide solution, boil, the active carbon that adds the 1.5-2.0% of medical material weight boils, and filters while hot, regulates pH value to 7.5-7.8 with 20% sodium hydroxide solution again, filter, embedding, sterilization, and get final product.
8. a method for preparing each described injection of claim 1-7 is characterized in that, the method may further comprise the steps:
1) Radix Astragali decocts with water 2-3 time, and collecting decoction filters, and is concentrated, adds ethanol and makes that to contain amount of alcohol be 70-75%, filter, and Recycled ethanol, thin up gets water extraction liquid, reclaims medicinal residues;
2) medicinal residues that reclaim alcohol reflux 2 times, merge extractive liquid,, Recycled ethanol, thin up gets alcohol extract;
3) merge water extraction liquid and alcohol extract, add ethanol and make and contain the alcohol amount and be 83%-87%, each all cold preservation is placed, and filters, and Recycled ethanol is to without the alcohol flavor, and thin up is regulated pH value, adds activated carbon adsorption, adds water to amount of preparation, filter, and embedding, sterilization, and get final product.
9. the application of each described injection of claim 1-7 in preparation treatment myocarditis, myocardial ischemia, heart failure, myocardial infarction, ARR medicine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210422499.6A CN102895294B (en) | 2012-10-30 | 2012-10-30 | Astragalus mongholicus injection and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210422499.6A CN102895294B (en) | 2012-10-30 | 2012-10-30 | Astragalus mongholicus injection and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102895294A true CN102895294A (en) | 2013-01-30 |
| CN102895294B CN102895294B (en) | 2014-09-03 |
Family
ID=47567980
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210422499.6A Active CN102895294B (en) | 2012-10-30 | 2012-10-30 | Astragalus mongholicus injection and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102895294B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104147030A (en) * | 2013-05-14 | 2014-11-19 | 天士力制药集团股份有限公司 | Protection effects of Astragaloside on heart |
| CN104997802A (en) * | 2014-04-25 | 2015-10-28 | 西安世纪盛康药业有限公司 | Pharmaceutical composition containing calycosin and pharmaceutical application thereof |
| CN106236820A (en) * | 2016-08-26 | 2016-12-21 | 黑龙江珍宝岛药业股份有限公司 | A kind of Radix Astragali injection and preparation method thereof and pharmaceutical composition |
| CN106619794A (en) * | 2016-12-27 | 2017-05-10 | 神威药业集团有限公司 | Refining method of high-stability radix astragali seu hedysari injection solution and radix astragali seu hedysari injection solution |
| CN108785370A (en) * | 2017-05-05 | 2018-11-13 | 中国科学院上海药物研究所 | A kind of pharmaceutical composition for treating hyperlipemia and atherosclerosis |
| CN113546073A (en) * | 2021-08-18 | 2021-10-26 | 广州医科大学附属第二医院 | Application of calycosin as TGFBR1 inhibitor in preparation of medicine for treating ventricular remodeling and myocardial fibrosis |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273116A (en) * | 1999-05-05 | 2000-11-15 | 方同华 | Process for refining astragalus injection |
| CN1515295A (en) * | 2003-01-08 | 2004-07-28 | 上海盛平医药科技有限公司 | Astragalus root extract injection and its preparation method |
-
2012
- 2012-10-30 CN CN201210422499.6A patent/CN102895294B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273116A (en) * | 1999-05-05 | 2000-11-15 | 方同华 | Process for refining astragalus injection |
| CN1515295A (en) * | 2003-01-08 | 2004-07-28 | 上海盛平医药科技有限公司 | Astragalus root extract injection and its preparation method |
Non-Patent Citations (3)
| Title |
|---|
| 《中成药》 20111130 简龙海等 黄芪注射液定性定量方法的改进 摘要，第2020页表2 4-9 第33卷, 第11期 * |
| 承燕等: "黄芪甲苷对心血管保护功能的研究进展", 《医学研究生学报》 * |
| 简龙海等: "黄芪注射液定性定量方法的改进", 《中成药》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104147030A (en) * | 2013-05-14 | 2014-11-19 | 天士力制药集团股份有限公司 | Protection effects of Astragaloside on heart |
| CN104997802A (en) * | 2014-04-25 | 2015-10-28 | 西安世纪盛康药业有限公司 | Pharmaceutical composition containing calycosin and pharmaceutical application thereof |
| CN106236820A (en) * | 2016-08-26 | 2016-12-21 | 黑龙江珍宝岛药业股份有限公司 | A kind of Radix Astragali injection and preparation method thereof and pharmaceutical composition |
| CN106619794A (en) * | 2016-12-27 | 2017-05-10 | 神威药业集团有限公司 | Refining method of high-stability radix astragali seu hedysari injection solution and radix astragali seu hedysari injection solution |
| CN106619794B (en) * | 2016-12-27 | 2020-08-21 | 神威药业集团有限公司 | Refining method of high-stability astragalus injection and astragalus injection |
| CN108785370A (en) * | 2017-05-05 | 2018-11-13 | 中国科学院上海药物研究所 | A kind of pharmaceutical composition for treating hyperlipemia and atherosclerosis |
| CN113546073A (en) * | 2021-08-18 | 2021-10-26 | 广州医科大学附属第二医院 | Application of calycosin as TGFBR1 inhibitor in preparation of medicine for treating ventricular remodeling and myocardial fibrosis |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102895294B (en) | 2014-09-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102895294B (en) | Astragalus mongholicus injection and preparation method thereof | |
| CN102600219B (en) | Total flavone extract of abelmoschus manihot and preparing method of total flavone extract | |
| CN101337000A (en) | Solanum nigrum extract, preparation method and use thereof | |
| CN101375990B (en) | Composition for treating cardiovascular disease and preparation thereof | |
| CN102119964B (en) | A kind of prevention and the extract for the treatment of angina pectoris, their Preparation method and use | |
| CN101306077B (en) | Chinese traditional injection preparation for treating cancer and its preparation method | |
| CN101337001B (en) | Solanum xanthocarpum extract, preparation method and use thereof | |
| CN1923241B (en) | Medicine composition containing epimedium extract, uncaria extract, and gastrodine, and its preparation and use | |
| CN101537036A (en) | Soap pod saponin extract as well as preparation method and application thereof | |
| CN101006984B (en) | An injection preparation containing salvianolic acid A and extract of panax natoginseng, and its preparation method and application | |
| CN101623437B (en) | Pulse-activating preparation for injection and preparation method thereof | |
| CN104945532B (en) | The preparation method of Gynura divaricata polysaccharide | |
| CN112159451A (en) | Gynostemma pentaphylla saponin extract and preparation method thereof | |
| CN101538297A (en) | Preparation method of high-purity monomer flavone and general flavone contained in capsella bursa-pastoris and application of general flavone | |
| CN101396373B (en) | Cinobufacini extract and preparation method thereof | |
| CN103463201B (en) | Extraction method of Shuanghuanglian extract | |
| CN103372034A (en) | Preparation method of ginkgo biloba extract | |
| CN101293009A (en) | Pharmaceutical composition | |
| CN103655653A (en) | Application of macroporous weakly acidic rosin based cationic exchange resin to adsorption of toxic ingredients in panax notoginseng saponins | |
| CN100584345C (en) | Distillage of Ardisia chinensis Benth of possessing function of antivirus, extraction method and application | |
| CN102085226B (en) | Japanese picris japonica extract and extracting method thereof | |
| CN101292987B (en) | Pharmaceutical combination | |
| CN101445544B (en) | Method for preparing ginsenoside Rb<1> | |
| CN110559327B (en) | Liver-protecting product and preparation method thereof | |
| CN101288705B (en) | Medicine composition mainly for adjusting blood fat and its preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160722 Address after: 158400 Hulin Red Star Street, Heilongjiang, No. 72 Patentee after: Heilongjiang ZBD Pharmaceutical Co., Ltd. Patentee after: Haerbin Zhenbao Pharmaceutical Co., Ltd. Address before: 158400 Hulin Red Star Street, Heilongjiang, No. 72 Patentee before: Heilongjiang ZBD Pharmaceutical Co., Ltd. |