CN105560173A - Highly stable Radix Astragali injection and preparation method thereof - Google Patents
Highly stable Radix Astragali injection and preparation method thereof Download PDFInfo
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- CN105560173A CN105560173A CN201511019116.0A CN201511019116A CN105560173A CN 105560173 A CN105560173 A CN 105560173A CN 201511019116 A CN201511019116 A CN 201511019116A CN 105560173 A CN105560173 A CN 105560173A
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- 239000009636 Huang Qi Substances 0.000 title claims abstract description 58
- 238000002347 injection Methods 0.000 title claims abstract description 32
- 239000007924 injection Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000243 solution Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 239000003814 drug Substances 0.000 claims description 31
- 238000004321 preservation Methods 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 229940079593 drug Drugs 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 20
- 239000012530 fluid Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000008215 water for injection Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 230000001954 sterilising effect Effects 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 3
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- HKQYGTCOTHHOMP-UHFFFAOYSA-N formononetin Chemical compound C1=CC(OC)=CC=C1C1=COC2=CC(O)=CC=C2C1=O HKQYGTCOTHHOMP-UHFFFAOYSA-N 0.000 abstract description 18
- 239000012535 impurity Substances 0.000 abstract description 11
- RIKPNWPEMPODJD-UHFFFAOYSA-N formononetin Natural products C1=CC(OC)=CC=C1C1=COC2=CC=CC=C2C1=O RIKPNWPEMPODJD-UHFFFAOYSA-N 0.000 abstract description 9
- 229930003935 flavonoid Natural products 0.000 abstract description 7
- 150000002215 flavonoids Chemical class 0.000 abstract description 7
- 235000017173 flavonoids Nutrition 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000003809 water extraction Methods 0.000 abstract description 3
- 238000003916 acid precipitation Methods 0.000 abstract 1
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- 238000009835 boiling Methods 0.000 abstract 1
- 238000005057 refrigeration Methods 0.000 abstract 1
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- 230000000052 comparative effect Effects 0.000 description 18
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- 239000004615 ingredient Substances 0.000 description 5
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- QMNWISYXSJWHRY-YLNUDOOFSA-N astragaloside IV Chemical compound O1[C@H](C(C)(O)C)CC[C@]1(C)[C@@H]1[C@@]2(C)CC[C@]34C[C@]4(CC[C@H](O[C@H]4[C@@H]([C@@H](O)[C@H](O)CO4)O)C4(C)C)[C@H]4[C@@H](O[C@H]4[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O4)O)C[C@H]3[C@]2(C)C[C@@H]1O QMNWISYXSJWHRY-YLNUDOOFSA-N 0.000 description 2
- QMNWISYXSJWHRY-BCBPIKMJSA-N astragaloside IV Natural products CC(C)(O)[C@@H]1CC[C@@](C)(O1)[C@H]2[C@@H](O)C[C@@]3(C)[C@@H]4C[C@H](O[C@@H]5O[C@H](CO)[C@H](O)[C@@H](O)[C@H]5O)[C@H]6C(C)(C)[C@H](CC[C@@]67C[C@@]47CC[C@]23C)O[C@@H]8OC[C@@H](O)[C@H](O)[C@H]8O QMNWISYXSJWHRY-BCBPIKMJSA-N 0.000 description 2
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- PFKIBRPYVNVMRU-UHFFFAOYSA-N cyclosieversioside F Natural products CC(C)(O)C1COC(C)(C1)C2C(O)CC3(C)C4CC(OC5OC(CO)C(O)C(O)C5O)C6C(C)(C)C(CCC67CC47CCC23C)OC8OCC(O)C(O)C8O PFKIBRPYVNVMRU-UHFFFAOYSA-N 0.000 description 2
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- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
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- 241001061264 Astragalus Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
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- 239000001263 FEMA 3042 Substances 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
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- 238000003556 assay Methods 0.000 description 1
- 235000006533 astragalus Nutrition 0.000 description 1
- 210000003719 b-lymphocyte Anatomy 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- WACBUPFEGWUGPB-MIUGBVLSSA-N calycosin-7-O-beta-D-glucoside Chemical compound C1=C(O)C(OC)=CC=C1C1=COC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)=CC=C2C1=O WACBUPFEGWUGPB-MIUGBVLSSA-N 0.000 description 1
- WACBUPFEGWUGPB-UHFFFAOYSA-N calycosin-7-O-beta-D-glucoside Natural products C1=C(O)C(OC)=CC=C1C1=COC2=CC(OC3C(C(O)C(O)C(CO)O3)O)=CC=C2C1=O WACBUPFEGWUGPB-UHFFFAOYSA-N 0.000 description 1
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- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 210000004233 talus Anatomy 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
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- 230000000304 vasodilatating effect Effects 0.000 description 1
- 230000003612 virological effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/08—Solutions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/481—Astragalus (milkvetch)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0019—Injectable compositions; Intramuscular, intravenous, arterial, subcutaneous administration; Compositions to be administered through the skin in an invasive manner
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Dermatology (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
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Abstract
The invention relates to the field of medicinal preparations, and concretely relates to a Radix Astragali injection and a preparation method thereof. The method comprises the following steps: carrying out water extraction and alcohol precipitation on Radix Astragali, carrying out acid precipitation treatment on the obtained alcohol precipitated liquid, adjusting the pH value to 7-8, preferably 7.5, by using an alkali, heating the obtained solution until boiling, refrigerating and disposing the boiled solution, and filtering the disposed solution to obtain the Radix Astragali injection. The above simple alcohol precipitated liquid pH value adjusting step is carried out to remove acidic impurities, and heat treatment, refrigeration and filtration are carried out to remove heat-insoluble impurities and ensure maximal reservation of effective components in the Radix Astragali. The preparation method solves the turbidity problem in the storage process of the Radix Astragali injection, avoids loss of the content of active actives, and maximally reserves the content of saponins and flavonoids, and especially the content of formononetin in the flavonoids.
Description
Technical field
The present invention relates to a kind of field of traditional Chinese, particularly a kind of high stability 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 while improving cardiac systolic function; still myocardium protecting action is had except heart failure effect; hypoxic-ischemic, ischemia-reperfusion can be protected and infect viral cardiac muscle, and the electrical activity of myocardial cell can be improved, and there is the effects such as arteriosclerosis.Radix Astragali extractive solution be a kind of there is Yiqiyangyuan, strengthening vital QI to eliminate pathogenic factors, nourish heart promote blood circulation, the Chinese herbal medicine of invigorating spleen to remove dampness effect, be usually used in that the motive is deficient, the hepatitis of the viral myocarditis of blood-vessel obstructive, cardiac insufficiency and stagnation of dampness due to deficiency of the spleen.Astrageloside has protection blood vessel endothelium, improves the effects such as hemorheology, can obviously promote B cell proliferation to break up and the synthesis of plasma cell antibody; In the arrhythmia that Radix Astragali total flavones class causes at acute myocardial infarction, viral myocarditis and barium chloride, there is protective effect.Therefore this two large class main component makes the Radix Astragali in Cardiovarscular, have significant curative effect.
In existing disclosed technology, the preparation method of Radix Astragali injection is disclosed: the Radix Astragali decocts with water three times in Traditional Chinese medicine historical preparation the 17, collecting decoction, filtrate concentrates, with alcohol settling process secondary, containing amount of alcohol in solution is for the first time 75%, second time is 85%, each all cold preservation is placed, reclaim ethanol and be concentrated into every 1ml and be 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 places 12 hours, filter, filtrate is concentrated into every 1ml and is equivalent to crude drug 5 ~ 6g, let cool, by 20% sodium hydroxide solution adjust ph to 7.5, boil, add the active carbon of 0.125%, boil 5 minutes, filter while hot, inject and make into 1000ml with water, filter, use 20% sodium hydroxide solution adjust ph to 7.5 again, filter, embedding, sterilizing, obtain.And mainly adopt the technique such as water extraction, precipitate with ethanol, upper resin column, enzyme hydrolysis, supercritical extraction to extract and the purification Radix Astragali in disclosed patent application at present.
Current astragalus extraction preparation technology also exists the problems such as precipitate with ethanol impurity-eliminating effect difference, and cause injection stabilizing effect poor, its effect duration reaches and namely easily produces medicinal liquid muddiness and occur opalescence half a year to 1 year.The principle active component of the Radix Astragali is the large class of soaping agents and flavonoid two.Also have polysaccharide, amino acids etc. in addition.After absorption with macroporous adsorbent resin remove impurity, although Radix Astragali injection can be solved deposit in process problem of becoming turbid, but effective ingredient soaping agents and flavonoid decline to a great extent, use the Chinese medicine preparation of this explained hereafter cannot reach the synergism of two large effective constituents, cause the reduction of curative effect.
Summary of the invention
The problem that the present invention mainly solves solves Radix Astragali injection to deposit in process problem of becoming turbid, and avoid Content of Astragaloside IV loss.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A preparation method for high stability Radix Astragali injection, carries out the heavy process of acid to gained alcohol deposit fluid after the Radix Astragali being carried out water extract-alcohol precipitation, and regulate pH to 7 ~ 8 (preferably 7.5), heated and boiled with alkali after sour heavy end, cold preservation is placed rear filtration and be get final product.
Method of the present invention, introduces the step that acid is heavy further after conventional water extract-alcohol precipitation terminates
Preferably, heavy the referring to of described acid utilizes acid solution to regulate described alcohol deposit fluid pH value to 1 ~ 2, described acid solution preferred salt acid solution.Farthest acid impurities can be removed in this pH value range.
Wherein, the mass concentration of described hydrochloric acid solution is 15 ~ 30%; Preferably 20%.
Preferably, described alkali is sodium hydroxide solution, carries out pH value adjustment with sodium hydroxide solution.
Further, the mass concentration of described sodium hydroxide solution is 15 ~ 30%; Preferably 20%.
Preferably, the time of described heated and boiled was at 60 ~ 80 minutes.Method of the present invention, can remove thermal instability impurity by further heated and boiled.
Preferably, cold preservation 10 ~ 15 hours at cold preservation of the present invention is placed in 2 ~ 10 DEG C, preferably cold preservation 12 hours at 4 ~ 8 DEG C, above-mentioned refrigerated condition contributes to contamination precipitation.
Find after deliberation; the Radix Astragali after water extraction, precipitate with ethanol still some acid impurities as tannic acid; acid impurities cannot be removed when extracting solution meta-alkali; although upper resin column can remove related impurities; but Radix Astragali effective ingredient also loses a lot; and the present invention can remove acid impurities by the simple alcohol deposit fluid pH value step that regulates, filtered by heat treatment cold preservation simultaneously and remove thermal instability impurity, can also to guarantee in the Radix Astragali simultaneously effective ingredient also retain to the limit.
Method of the present invention, also comprise and place to cold preservation further and in filtrate after filtering, add the active carbon of 0.1% ~ 0.15%, boil 2 ~ 10 minutes, filter while hot, inject water to recipe quantity, filter, use sodium hydroxide solution adjust ph to 7.5 again, filter, embedding, sterilizing, obtains described high stability Radix Astragali injection.
Above-mentioned steps is more conducive to the quality controlling Radix Astragali injection of the present invention.
Above-mentioned " recipe quantity " is grasped by those skilled in the art, and if every 2000g Radix Astragali is as raw material, it is 1000ml that the consumption of water for injection preferably adds to full dose.
Method of the present invention, wherein " water extract-alcohol precipitation " can adopt ordinary skill in the art means, and as preferably, described water extract-alcohol precipitation is specially:
(1) get the Radix Astragali, decoct with water 2 ~ 4 times, collecting decoction, decocting liquid is concentrated into every 1ml and is equivalent to crude drug 1 ~ 2g;
(2) with alcohol settling process 1 ~ 3 time, cold preservation is placed, and merges heavy liquid, reclaims ethanol and be concentrated into every 1ml to be equivalent to crude drug 10g;
(3) be diluted to every 1ml with water for injection and be equivalent to crude drug 0.75 ~ 1g, 10-15 hour is placed in cold preservation, and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug 5 ~ 6g, lets cool, and obtains described alcohol deposit fluid.
The concrete operations of above-mentioned water extract-alcohol precipitation contribute to the enrichment of astragaloside and formononetin.
As preferred forms of the present invention, the preparation method of high stability Radix Astragali injection of the present invention comprises the following steps:
(1) get Radix Astragali 2000g, decoct with water 3 times, collecting decoction, decocting liquid is concentrated into every 1ml and is equivalent to crude drug 1 ~ 2g;
(2) with alcohol settling process 2 times, containing amount of alcohol in solution is for the first time 75%, and second time is 85%, each all cold preservation placement, the heavy liquid of merging, reclaims ethanol and be concentrated into every 1ml to be equivalent to crude drug 10g;
(3) be diluted to every 1ml with water for injection and be equivalent to crude drug 0.75 ~ 1g, cold preservation places 12 hours, and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug 5 ~ 6g, lets cool, obtains alcohol deposit fluid;
(4) described alcohol deposit fluid pH value to 1 ~ 2 are regulated, cold preservation, filtration with 20% hydrochloric acid solution, by 20% sodium hydroxide solution adjust ph to 7.5;
(5) heated and boiled 60 minutes, at 4 ~ 8 DEG C, cold preservation places 12 hours, filters;
(6) add the active carbon of 0.125%, boil 5 minutes, filter while hot, inject water to recipe quantity, filter, then use 20% sodium hydroxide solution adjust ph to 7.5, filter, embedding, sterilizing, to obtain final product.
Adopt technique scheme, by increasing, acid is heavy, heat treatment cold preservation is filtered two steps and can be removed impurity completely in the present invention, and effective ingredient astragaloside etc. is at utmost retained.The invention solves Radix Astragali injection and deposit in process problem of becoming turbid, avoid the loss of active component content, remain soaping agents and Flavone content to greatest extent, the formononetin content especially in flavonoid.
The Radix Astragali injection that the present invention protects said method to prepare simultaneously.
In above-mentioned Radix Astragali injection, the astragaloside of every 1ml must not be less than 0.08mg, and formononetin content is no less than 0.12mg/ml.
Radix Astragali injection of the present invention has the feature of high activity content and high stability, more known Radix Astragali injection contains higher astragaloside, flavonoids effective constituent content and more preferably stability, not only solve Radix Astragali injection and deposit in process problem of becoming turbid, and remain soaping agents and Flavone content to greatest extent, especially the formononetin content in flavonoid, formononetin has antibacterial and estrogen-like effects, is one of the effective ingredient of the Radix Astragali.
Detailed description of the invention
Below by way of concrete preferred embodiment, the present invention is further described.These embodiments are only illustrative, and should not be construed as limitation of the present invention.
In following examples, involved all raw materials are known commercially available prod.
Embodiment 1
Present embodiments provide a kind of Radix Astragali injection, its preparation method comprises the following steps:
(1) get Radix Astragali 2000g, decoct with water 3 times, collecting decoction, filtrate is concentrated into every 1ml and is equivalent to crude drug 1 ~ 2g.
(2) with alcohol settling process 2 times, be 75% containing amount of alcohol in first time solution, second time is 85%, and each all cold preservation is placed, and reclaims ethanol and be concentrated into every 1ml to be equivalent to crude drug 10g.
(3) be diluted to every 1ml with water for injection and be equivalent to crude drug 0.75 ~ 1g, cold preservation places 12 hours, and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug 5 ~ 6g, lets cool, obtains alcohol deposit fluid.
(4) described alcohol deposit fluid pH value to 1.5 is regulated, cold preservation, filtration with 20% hydrochloric acid solution, by 20% sodium hydroxide solution adjust ph to 7.5.
(5) heated and boiled 60 minutes, at 4 ~ 8 DEG C, cold preservation places 12 hours, filters.
(6) add the active carbon of 0.125%, boil 5 minutes, filter while hot, inject water to 1000ml, filter, then use 20% sodium hydroxide solution adjust ph to 7.5, filter, embedding, sterilizing, to obtain final product.
Embodiment 2
Present embodiments provide a kind of Radix Astragali injection, compared with embodiment 1, distinctive points is only: use the hydrochloric acid solution of 15% and the sodium hydroxide solution adjust ph of 15% in step (4) respectively in the present embodiment, and in the heavy process of acid, control ph is 1.
Embodiment 3
Present embodiments provide a kind of Radix Astragali injection, compared with embodiment 1, distinctive points is only: use the hydrochloric acid solution of 30% and the sodium hydroxide solution adjust ph of 30% in step (4) respectively in the present embodiment, and in the heavy process of acid, control ph is 2.
Embodiment 4
Present embodiments provide a kind of Radix Astragali injection, compared with embodiment 1, distinctive points is only: being prepared as follows of alcohol deposit fluid:
(1) get Radix Astragali 2000g, decoct with water 2 times, collecting decoction, filtrate is concentrated into every 1ml and is equivalent to crude drug 1 ~ 2g.
(2) with alcohol settling process 3 times, be 75% containing amount of alcohol in first time solution, second and third time is 85%, and each all cold preservation is placed, and reclaims ethanol and be concentrated into every 1ml to be equivalent to crude drug 10g.
(3) be diluted to every 1ml with water for injection and be equivalent to crude drug 0.75 ~ 1g, cold preservation places 15 hours, and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug 5 ~ 6g, lets cool, obtains alcohol deposit fluid.
Comparative example 1
This comparative example is compared with embodiment 1, and distinctive points is only, this comparative example adopts ministry standard technique to extract the Radix Astragali, and concrete technique is see Traditional Chinese medicine historical preparation the 17.
Comparative example 2
This comparative example is compared with embodiment 1, and distinctive points is only, this comparative example employing publication number is the open technique of China's application of CN101049339.
Comparative example 3
This comparative example is compared with embodiment 1, and distinctive points is only, this comparative example is without step 4 (namely acid is heavy).
Comparative example 4
This comparative example is compared with embodiment 1, and distinctive points is only, this comparative example is without step 5.
Comparative example 5
This comparative example is compared with embodiment 1, and distinctive points is only, in step 4, in the heavy process of acid, pH value controls to be 4.
The Radix Astragali injection quality of comparative example 1-3 and comparative example 1-5 gained, wherein, Content of Astragaloside IV assay method can with reference to Traditional Chinese medicine historical preparation the 17 Radix Astragali injection quality standard, the content assaying method of formononetin can the list of references content of Calycosin-7-O-BETA-D-glucoside and formononetin " in the high effective liquid chromatography for measuring Radix Astragali " (Ji Songgang etc. The 2nd Army Medical College journal .2006,27:81-84, comparing result is in table 1.
The different extraction process of table 1 is on the impact of Radix Astragali injection clarity and content
Result shows: compared with comparative example, and Radix Astragali injection provided by the invention still conforms with the regulations in long-term investigation 12 clarity in the middle of the month, and the content of principle active component astragaloside, formononetin is obviously higher.Although Radix Astragali injection long-term investigation 12 clarity in the middle of the month that comparative example 2 is produced conforms with the regulations, owing to adopting upper prop technique, principle active component content is obviously lower.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. a preparation method for high stability Radix Astragali injection, is characterized in that: carry out the heavy process of acid to gained alcohol deposit fluid after the Radix Astragali being carried out water extract-alcohol precipitation, and regulate pH to 7 ~ 8, heated and boiled with alkali after sour heavy end, cold preservation is placed rear filtration and be get final product.
2. preparation method according to claim 1, is characterized in that: heavy the referring to of described acid utilizes acid solution to regulate described alcohol deposit fluid pH value to 1 ~ 2, described acid solution preferred salt acid solution.
3. preparation method according to claim 2, is characterized in that: the mass concentration of described hydrochloric acid solution is 15 ~ 30%, preferably 20%.
4. the preparation method according to any one of claims 1 to 3, is characterized in that: described alkali is sodium hydroxide solution, and the mass concentration of preferred described sodium hydroxide solution is 15 ~ 30%, more preferably 20%.
5. the preparation method according to any one of Claims 1 to 4, is characterized in that: the time of described heated and boiled was at 60 ~ 80 minutes.
6. the preparation method according to any one of Claims 1 to 5, is characterized in that: cold preservation 10 ~ 15 hours at described cold preservation is placed in 2 ~ 10 DEG C, preferably 12 hours.
7. the preparation method according to any one of claim 1 ~ 6, it is characterized in that: described method also comprises places to cold preservation further and adds the active carbon of 0.1% ~ 0.15% in filtrate after filtering, boil 2 ~ 10 minutes, filter while hot, inject water to recipe quantity, filter, use sodium hydroxide solution adjust ph to 7.5 again, filter, embedding, sterilizing, obtains described high stability Radix Astragali injection.
8. the preparation method according to any one of claim 1 ~ 7, is characterized in that: described water extract-alcohol precipitation is specially:
(1) get the Radix Astragali, decoct with water 2 ~ 4 times, collecting decoction, decocting liquid is concentrated into every 1ml and is equivalent to crude drug 1 ~ 2g;
(2) with alcohol settling process 1 ~ 3 time, cold preservation is placed, and merges heavy liquid, reclaims ethanol and be concentrated into every 1ml to be equivalent to crude drug 10g;
(3) be diluted to every 1ml with water for injection and be equivalent to crude drug 0.75 ~ 1g, cold preservation is placed 10 ~ 15 hours, and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug 5 ~ 6g, lets cool, and obtains described alcohol deposit fluid.
9. preparation method according to claim 1, is characterized in that: described in comprise the following steps:
(1) get Radix Astragali 2000g, decoct with water 3 times, collecting decoction, decocting liquid is concentrated into every 1ml and is equivalent to crude drug 1 ~ 2g;
(2) with alcohol settling process 2 times, containing amount of alcohol in solution is for the first time 75%, and second time is 85%, each all cold preservation placement, the heavy liquid of merging, reclaims ethanol and be concentrated into every 1ml to be equivalent to crude drug 10g;
(3) be diluted to every 1ml with water for injection and be equivalent to crude drug 0.75 ~ 1g, cold preservation places 12 hours, and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug 5 ~ 6g, lets cool, obtains alcohol deposit fluid;
(4) described alcohol deposit fluid pH value to 1 ~ 2 are regulated, cold preservation, filtration with 20% hydrochloric acid solution, by 20% sodium hydroxide solution adjust ph to 7.5;
(5) heated and boiled 60 minutes, at 4 ~ 8 DEG C, cold preservation places 12 hours, filters;
(6) add the active carbon of 0.125%, boil 5 minutes, filter while hot, inject water to 1000ml, filter, then use 20% sodium hydroxide solution adjust ph to 7.5, filter, embedding, sterilizing, to obtain final product.
10. the high stability Radix Astragali injection for preparing of preparation method described in any one of claim 1-9.
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