CN1935230B

CN1935230B - Chinese medicine injection preparation and its preparing method

Info

Publication number: CN1935230B
Application number: CN200610111673XA
Authority: CN
Inventors: 于文风
Original assignee: Qiyuanyide Medicines Institute Beijing
Current assignee: Qiyuanyide Medicines Institute Beijing
Priority date: 2005-08-22
Filing date: 2006-08-22
Publication date: 2010-04-14
Anticipated expiration: 2026-08-22
Also published as: CN1935230A

Abstract

The present invention relates to a Chinese medicine injection preparation for raising immunity of body and curing angiocardiopathy and cerebrovascular disease. Said Chinese medicine injection preparation is made up by using the Chinese medicinal materials of ophiopogon tuber, ginseng or red ginseng or pilose asiabell root and erigeron breviscapus through a certain preparation process. Said Chinesemedicine injection preparation can obtain good therapeutic effect for curing the diseases of coronary heart disease, angina pectoris, arrhythmia, cenebral thrombosis and senile dementia, etc.

Description

A kind of traditional medicine Injectio and preparation method thereof

Technical field

The present invention is a kind of ejection preparation with human body immunity improving power, treatment cardiovascular and cerebrovascular disease and preparation method thereof, belongs to technical field of Chinese medicine.

Technical background

We's medical application---cardiovascular and cerebrovascular disease, as coronary heart disease, myocardial infarction, rhomboembolia type cerebrovascular etc. is sickness rate height, disability rate height and the also high disease of case fatality rate, with diabetes, tumor etc. is at present the mankind to be threatened maximum three major types disease, and wherein cardiovascular and cerebrovascular disease is positioned at first of this three big disease.There is 2,600,000 people every year in China because of cardiovascular and cerebrovascular disease death at present, so prevention and treatment cardiovascular and cerebrovascular disease have become a necessity and arduous problem.

The medicine that is used for the treatment of at present cardiovascular and cerebrovascular disease clinically is generally Radix Salviae Miltiorrhizae Injection, SHENGMAI ZHUSHEYE, SHENMAI ZHUSHEYE, Breviscapini injection etc., yet these injection curative effects are very not desirable, and the report that untoward reaction is all arranged, the clinical reports of delivering in " clinical misdiagnosis wrong treatment " the 6th phase of calendar year 2001 at the above " giving birth to the untoward reaction of arteries and veins (and ginseng arteries and veins) injection ", Li Lanqing etc. of " Chinese patent medicine " 1999 the 8th phases as Zhuan Zhiquan such as " untoward reaction of Herba Erigerontis injection ".The applicant thinks that the reason that produces this situation may be: 1, the prescription of these preparations and proportioning thereof have much room for improvement, effect such as Breviscapini injection, Radix Salviae Miltiorrhizae Injection is single, can only be to a certain cause of disease pathological changes generation effect of cardiovascular and cerebrovascular disease, so curative effect is undesirable; 2, the processing extraction is impure, and some compositions such as pigment, tannin, starch, protein etc. are remained in the medicinal liquid with colloidal form, thereby untoward reaction takes place.Effective ingredient in Chinese or effective part group have multiple composition synergism, make its performance better therapeutic.Therefore, invent a kind of good effect, untoward reaction few, to the cardiovascular and cerebrovascular disease Different types of etiopathogenises produce the medicament composing prescription of synergistic therapeutic action and preparation thereof, technology is necessary.

The applicant drafts prescription: Radix Ophiopogonis, Radix Ginseng, Herba Erigerontis from the medicine of several respects researchs such as Chinese medicine traditional theory, pathomechanism treatment cardiovascular and cerebrovascular disease.From Chinese medicine theoretically, Radix Ginseng QI invigorating reinforcing the heart; Radix Ophiopogonis YIN nourishing and the production of body fluid promoting, Fu Mai; Herba Erigerontis has the effect of dredge the meridian passage, blood circulation promoting and blood stasis dispelling, and three medicine compatibilities are combined into a kind of pharmaceutical preparation that can effectively treat cardiovascular and cerebrovascular disease.From pathomechanism, vascular lesion is the main cause that causes at present known all cardiovascular and cerebrovascular vessel incident, and can be divided into ischemic and hemorrhagic two big classes from lesion nature, and the former sickness rate is far above the latter.In recent years, the free radical mechanism research of ischemic heart and brain damage is very active, has obtained bigger progress in many aspects.Prior art shows the effect that has Herba Erigerontis, Radix Ginseng, Radix Ophiopogonis good removing reactive oxygen free radical.Inventor's process discovers that three's compatibility result of use is better than the single medicine, and through the drug effective region that the process for refining that the present invention studies prepares, active ingredient has been carried out rich long-pending and purification, thereby made the effect of preparation better.

Summary of the invention

The object of the present invention is to provide a kind of ejection preparation and preparation method thereof with human body immunity improving power, treatment cardiovascular and cerebrovascular disease; The present invention utilizes the Radix Ginseng strongly invigorating primordial QI, Radix Ophiopogonis YIN nourishing and the production of body fluid promoting, Herba Erigerontis relaxing muscles and tendons to promote blood circulation, analgesic effect are combined into a kind of preparation that can effectively treat cardiovascular and cerebrovascular disease.The present invention is directed to prior art,, adopt the mode of separately extracting at different medical materials, both can effectively extract active component, can under the situation that guarantees active component, remove impurity targetedly simultaneously, sample is made with extra care, make injection, make the faster performance curative effect of medicine performance, the bioavailability height is particularly useful for the treatment of cardiovascular and cerebrovascular disease acute attack stage, while preparation of the present invention is human body immunity improving power effectively, the generation of prevention and resist the disease.

Technical solution of the present invention is achieved in that

The present invention is a kind of traditional medicine Injectio with human body immunity improving power, treatment cardiovascular and cerebrovascular disease, calculate according to components by weight percent, it is made through extracting refining and adding suitable adjuvant by 50～5000 parts of 10～1000 parts of 10～1000 parts of Radix Ophiopogonis, Radix Ginseng and Herba Erigerontiss, or adds the injection that suitable adjuvant is made by corresponding weight portion medical material through extracting the refining extract that obtains; Say exactly, be to be made through extracting refining and adding suitable adjuvant, or add the injection that suitable adjuvant is made through extracting the extract that obtains after refining by corresponding weight portion medical material by 50～1000 parts of 10～500 parts of 10～500 parts of Radix Ophiopogonis, Radix Ginseng and Herba Erigerontiss; More preferably be made through extracting refining and adding suitable adjuvant, or add the injection that suitable adjuvant is made through extracting the extract that obtains after refining by corresponding weight portion medical material by 200～500 parts of 50～200 parts of 50～200 parts of Radix Ophiopogonis, Radix Ginseng and Herba Erigerontiss.Contain saponin component in the effective site Radix Ginseng total saponins of Radix Ginseng and be not less than 50%, contain saponin component in the effective site Radix Ophiopogonis total saponins of Radix Ophiopogonis and be not less than 50%, contain the polysaccharide composition in the another one effective site Radix Ophiopogonis polysaccharide of Radix Ophiopogonis and be not less than 50%, contain flavones ingredient in the effective site Herba Erigerontis total flavones of Herba Erigerontis and be not less than 50%; All can survey saponin component in the preparation, polysaccharide composition, flavones ingredient and other the composition sum and account for that the total solid after the deduction adjuvant amount and water quantities is not less than 25% in the preparation.

Contain various saccharides compositions such as Radix Ophiopogonis polysaccharide and monosaccharide in the preparation, calculate according to percentage by weight, the content of carbohydrate content accounts for that the total solid after the deduction adjuvant amount and water quantities is not less than 4% in the preparation.Also contain saponin component, polysaccharide composition and flavones ingredient in the preparation, calculate according to percentage by weight, wherein the content of saponin component accounts for that the total solid after the deduction adjuvant amount and water quantities is not less than 1% in the preparation; The total solid that the content of flavones ingredient accounts in the preparation after deduction adjuvant amount and the water quantities is not less than 1%, and what the content of polysaccharide composition accounted for the total solid after the deduction adjuvant amount and water quantities in the preparation is not less than 3%.

Injection of the present invention comprises: be directly used in drug administration by injection injection, need to be used for the concentrated solution for injection of intravenous drip after the dilution, directly for the venous transfusion of intravenous drip and injectable sterile powder and the aseptic block that makes with freeze-drying or spray drying method.

Drug effective region of the present invention can be commercially available or adopt following method preparation:

Radix Ophiopogonis, people participate in Herba Erigerontis three flavor medical materials and add water or ethanol extraction respectively, extracting solution carry out suitably concentrating crude extract and further adopt one or more methods in alcohol deposition method, water precipitating method, acid-base precipitation method, flocculent precipitation, column chromatography, the organic solvent extractionprocess be used in combination refining extract, the refining extract of get it filled material crude extract or medical material adds adjuvant and makes different ejection preparations.

The preparation of preparation of the present invention can be adopted method:

A, get medical material Radix Ophiopogonis, adding 5～15 times of volume decoctings boils 1～4 time, each 0.5～2.5 hour, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.3-0.8ml/g medical material min, water with 3-10 times of resin volume washes with the speed of 0.5-1.5ml/g medical material min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 50～70%, make for the second time that to contain the alcohol amount be 80～90%, filter, twice precipitation merged the back add 1～4 times of water dissolution, filter, filtrate concentrate Radix Ophiopogonis polysaccharide, the 5-25% ethanol of reuse 1-4 times of resin volume is with the speed eluting impurity of 0.5-1.5ml/g medical material min, at last with the 50-70% ethanol of 2-6 times of resin volume speed eluting with 0.5-1.0ml/g medical material min, collect stripping liquid, get Radix Ophiopogonis total saponins and the merging of above-mentioned Radix Ophiopogonis polysaccharide after reclaiming ethanol, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 5～15 times of volume 50～80% alcohol reflux 1～4 time, each 0.5～2.5 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 1-5 times of medical material volume, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.1-0.8ml/g medical material min, with 1-10 times of resinite hydrops and 1-6 times of resin volume 5-15% alcohol flushing impurity, with the 30-70% alcohol desorption of 1-7 times of resin volume, collect stripping liquid then successively, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the ginseng crude drug, add 5～15 times of volume 50～80% alcohol reflux 1～4 time, each 0.5～2.5 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 1-5 times of medical material volume, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 0.3-1.5ml/g medical material min, with 1-10 times of resinite hydrops and 1-6 times of resin volume 5-15% alcohol flushing impurity, with the 30-70% alcohol desorption of 1-7 times of resin volume, collect stripping liquid then successively, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add adjuvant and make different ejection preparations.

The preparation method of preparation of the present invention is specially:

A, get medical material Radix Ophiopogonis, adding 8 times of volume decoctings boils 3 times, each 1 hour, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.5ml/g medical material min, water with 6 times of resin volumes washes with the speed of 1ml/g medical material min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, the-inferiorly make that to contain the alcohol amount be 60%, make for the second time that to contain the alcohol amount be 85%, filter, will twice precipitation merge the back and add 2 times of water dissolutioies, filter, measuring relative density when filtrate decompression is concentrated into 60 ℃ is 1.05～1.15, gets Radix Ophiopogonis polysaccharide, and 20% ethanol of 3 times of resin volumes of reuse is with the speed eluting impurity of 1ml/g medical material min, use the speed eluting of 60% ethanol of 4 times of resin volumes at last with 0.8ml/g medical material min, collect stripping liquid, get Radix Ophiopogonis total saponins and the merging of above-mentioned Radix Ophiopogonis polysaccharide behind the recovery ethanol, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 3 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.2ml/g medical material min, use 5 times of resinite hydrops and 4 times of resin volume 10% alcohol flushing impurity successively, use 40% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry the thin total flavones of oil lamp;

C, get the ginseng crude drug, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 4 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 1ml/g medical material min, use 7 times of resinite hydrops and 5 times of resin volume 10% alcohol flushing impurity successively, use 60% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

Aseptic block in the injection of the present invention is preparation like this:

A, get medical material Radix Ophiopogonis, adding 8 times of volume decoctings boils 3 times, each 1 hour, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.5ml/g medical material min, water with 6 times of resin volumes washes with the speed of 1ml/g medical material min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 60%, make for the second time that to contain the alcohol amount be 85%, filter, will twice precipitation merge the back and add 2 times of water dissolutioies, filter, measuring relative density when filtrate decompression is concentrated into 60 ℃ is 1.05～1.15, gets Radix Ophiopogonis polysaccharide, and 20% ethanol of 3 times of resin volumes of reuse is with the speed eluting impurity of 1ml/g medical material min, use the speed eluting of 60% ethanol of 4 times of resin volumes at last with 0.8ml/g medical material min, collect stripping liquid, get Radix Ophiopogonis total saponins and the merging of above-mentioned Radix Ophiopogonis polysaccharide behind the recovery ethanol, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 3 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.2ml/g medical material min, use 5 times of resinite hydrops and 4 times of resin volume 10% alcohol flushing impurity successively, use 40% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 1.0% active carbon, boil, keep little 30min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, and adjust pH 5.5～7.5 boils, at 4 ℃ of cold preservations 12 hours, coarse filtration, fine straining.Suitable adjuvant is added the injection water is mixed with solution,, filter with above-mentioned filtrate mixing, packing, temperature-45 ℃, pre-freeze time 10h, the beginning evacuation, and in 12～72 hours differential gradient increased temperature to 10 ℃ progressively, keep 2h, be warming up to 20 ℃, keep 2h, promptly.

Injection with small volume in the injection of the present invention or concentrated solution for injection can prepare like this:

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 0.1%～1.5% active carbon, boil, keep little 10～60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 5.5～7.5, boil, 1～8 ℃ of cold preservation 12 hours, coarse filtration, fine straining, dividing to install in the ampoule bottle, is 100～110 ℃ in vapor (steam) temperature, and actual pressure is at 100～120kN/m ³Pressure sterilizing is 40～60 minutes under the condition, promptly gets the injection with small volume or the concentrated solution for injection that are directly used in drug administration by injection.

Glucose intravenous infusion agent in the injection of the present invention can prepare like this:

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, add the glucose of ormal weight again, by volume add 0.1%～1.5% active carbon, boil, keep little 10～60min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, transfer pH value 5.5～7.5, boil, at 1～8 ℃ of cold preservation 12 hours, coarse filtration, fine straining, add the injection water, packing is under 105～125 ℃ of conditions, sterilized 20～60 minutes, and promptly got the glucose intravenous infusion agent.

Sodium chloride intravenous infusion agent in the injection of the present invention can prepare like this:

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, add the sodium chloride of ormal weight again, by volume add 0.1%～1.5% active carbon, boil, keep little 10～60min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, transfer pH value 5.5～7.5, boil, at 1～8 ℃ of cold preservation 12 hours, coarse filtration, fine straining, add the injection water, packing is under 105～125 ℃ of conditions, sterilized 20～60 minutes, and promptly got the sodium chloride intravenous infusion agent.

Freeze dry sterile powder end in the injection of the present invention can prepare like this:

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 0.1%～1.5% active carbon, boil, keep little 10～60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfers pH value 5.5～7.5, boils, 1～8 ℃ of cold preservation 12 hours, coarse filtration, fine straining divide to install in the enamel tray, temperature-55～-45 ℃, pre-freeze time 8～12h, the beginning evacuation, and be warming up to-43～-37 ℃, keep 6～10h, be warming up to-33～-27 ℃ again, keep 6～10h; Be warming up to-23～-17 ℃, keep 6～10h, be warming up to-13～-7 ℃, keep 4～6h, be warming up to-3～3 ℃, keep 4～6h, be warming up to 7～13 ℃, keep 1～3h, be warming up to 17～23 ℃, keep 1～3h, under aseptic condition, divide to install to promptly to get the freeze dry sterile powder end in the cillin bottle.

Spray drying sterilized powder in the injection of the present invention can prepare like this:

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 0.1%～1.5% active carbon, boil, keep little 10～60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, adjust pH 5.5～7.5 boiled, 1～8 ℃ of cold preservation 12 hours, coarse filtration, fine straining, in inlet temperature is 140～160 ℃, and leaving air temp is 60～80 ℃, and air velocity is 16～20ms ^-1Condition under spray drying get powder, packing promptly gets the spray drying sterilized powder.

The adjuvant that is adopted in the preparation of the present invention comprises one or more in mannitol, galactose, glycine, glucose, sodium chloride, dextran, glycerol, ethanol, propylene glycol, Polyethylene Glycol, sorbitol, tween, the poloxamer.

Radix Ginseng involved in the present invention can also be the Radix Ginseng Rubra or the Radix Codonopsis of equivalent.Compared with prior art, salience progress of the present invention is:

The applicant filters out optimum prescription in conjunction with aspects such as traditional Chinese medicine theory, cardiovascular and cerebrovascular disease pathomechanism, each effective ingredient site of actions; make it possess effects such as the blood vessel of expansion, brain protection, anticoagulant, the healing of promotion myocardial damage; and respectively each flavor Effective Components of Chinese Herb is extracted; be prepared into compound preparation, pharmacodynamics test proves that this compound preparation has stronger curative effect to cardiovascular and cerebrovascular disease than other preparations and single medicinal substances extract.The three herbal medicine rational and effective prescription proportionings that the present invention filters out, can many-sided effect in the vascular lesion position, and enhancing human body immunity power had better effect.Find that simultaneously Herba Erigerontis, Radix Ophiopogonis, compatibility Radix Ginseng Rubra, Radix Codonopsis also had certain curative effect.

Each medical material of this prescription adopts and extracts separately and suitable process for refining, avoids occurring the complicated component that mixed extraction may cause, and the pigment that remove impurity does not totally cause, tannin, protein etc. remain in the medium problem of medicinal liquid.For example, the applicant finds that under study for action Herba Erigerontis adopts AB-8 macroporous resin column separating purification effective.

The applicant finds that in injection with small volume or concentrated solution for injection molding research the effective ingredient breviscapine dissolubility of Herba Erigerontis is low, and chemical stability problems appears in preparation easily.Through repetition test; we adopt the ethanol extraction Herba Erigerontis of higher concentration; and the medicinal liquid pH value is adjusted to 5.5～7.5; this moment, medicinal liquid was relatively stable; do not produce microgranule or any cosmetic variation; index components scutellarin content does not have too big variation, has effectively solved the problem of Herba Erigerontis stability.

Lyophilized formulations provided by the invention because main component is a polysaccharide material, situations such as spray bottle, lyophilizing are incomplete occurred in freezing dry process.Through our repetition test, adopt rational freeze-dry process, preferably resolve this difficult problem.The inventor finds that in research process most of adjuvant all can be made into freeze-dried powder, but solubility angle integrated survey from yield rate, molding situation and sample, use the effect of mannitol to be better than other several adjuvants separately, both can satisfy the every requirement of injection, and reduce simultaneously as far as possible and add too much adjuvant.

Experimentation shows, the prescription side effect that the applicant screened is little, cardiovascular and cerebrovascular disease is had tangible curative effect, and the formulation products that obtains is the good medicine of human body immunity improving power, treatment cardiovascular and cerebrovascular disease; The selected preparation technology of the present invention extracts the medical material effective ingredient when removing impurity; The selected moulding process of the present invention is rationally controlled.

The applicant has carried out a series of experiments, can prove that safety of medicine provided by the invention is effective, process stabilizing, quality controllable.

Experimental example 1: drug effectiveness research

The applicant has carried out following test, proves the curative effect of product of the present invention.

The pharmacological research conclusion

Of the present invention group of Herba Erigerontis injection group of pilot project

The myocardial infarction model test effect is remarkable due to the dog coronary artery ligation method, and the effect reinforced effects is general

The antiplatelet aggregation test effect is remarkable, and the effect reinforced effects is obvious

Anti-mouse tail thrombotest effect is remarkable, and the effect reinforced effects is general

Rabbit fibrin solubility test effect is obvious, and the effect reinforced effects is general

The test effect remarkable result of white mice normal pressure anoxia enduring time-to-live is not obvious

From above-mentioned test as can be seen, the combination preparation therapeutic effect is significantly better than single preparation group.

Experimental example 2: extraction process Study on Conditions

2.1 Herba Erigerontis Study on Preparation

Through above analysis and investigation, determined preparation technology's basic technology route.This test will be investigated the principal element that influences flavones ingredient extraction effect in the Herba Erigerontis, as extracting solvent, extraction time etc., to determine the preferred process condition.

2.1.1 the investigation of concentration of alcohol

According to the EXPERIMENTAL DESIGN of extraction process, Different concentrations of alcohol is carried out preferably.Design is respectively with 30%, 50% in the test, and 70%, 90% ethanol is as extracting solvent, serves as to investigate index with the rate of transform of scutellarin in the extract, in conjunction with the content of scutellarin, different extraction solvents investigated simultaneously.

Test method: take by weighing 4 parts of Herba Erigerontiss, every part of 300g pulverizes, and adds the different solvents of 10 times of volumes respectively, reflux, extract, 3 times, each 1 hour.Respectively extracting solution is filtered, decompression filtrate recycling ethanol (60 ℃) concentrates, vacuum drying (60 ℃ ,-0.09Mpa).Measure the content of scutellarin.

The investigation table of concentration of alcohol

Heavy (g) scutellarin content (%) rate of transform (%) of concentration of alcohol (%) medical material weight (g) cream

30 300.05 23.10 4.28 84.50

50 300.10 23.25 4.60 89.42

70 300.15 17.53 6.45 95.14

90 300.08 17.28 6.31 94.67

The result shows, during with 70% ethanol extraction, the scutellarin content and the rate of transform all are higher than the ethanol of other concentration.So the ethanol of selection 70% is as extracting solvent.

2.1.2 extraction conditions is preferred

After having determined the extraction solvent of Herba Erigerontis, also need extraction conditions is further carried out preferably.When extracting with heating reflux method, the principal element that influences extraction effect has: extraction time, solvent load and extraction time etc.Simultaneously can truly reflect result of the test again in order to reduce test number (TN), adopt the orthogonal experiment experiment arrangement.With extraction time, extraction time and solvent load is the investigation factor, and three levels of each factor design serve as to investigate index with the rate of transform of scutellarin, select L for use ₉(3 ⁴) orthogonal table, the Herba Erigerontis extraction conditions is carried out preferably.

Extract experimental factor level design table

Factor extraction time (hour) extraction time (inferior) ethanol consumption (doubly)

Horizontal A B C

1 0.5 1 8

2 1 2 10

3 1.5 3 12

Test method: take by weighing Herba Erigerontis 300g, totally 9 parts, according to L ₉(3 ⁴) each condition of orthogonal table refluxes, and collects extracting solution, 60 ℃ of decompression recycling ethanols, vacuum drying (60 ℃ ,-0.09Mpa), accurately weigh, measure scutellarin content.

The extraction conditions orthogonal test table

Factor

The A B C D rate of transform (%)

Level

1 1 1 1 1 75.53

2 1 2 2 2 82.2

3 1 3 3 3 90.33

4 2 1 2 3 81.9

5 2 2 3 1 87.92

6 2 3 1 2 92.04

7 3 1 3 2 80.89

8 3 2 1 3 86.73

9 3 3 2 1 93.35

I 248.06 238.32 254.3 256.8

II 261.86 256.85 257.45 255.13

III 260.97 275.72 259.14 258.96

I 82.69 79.44 84.77 85.60

II 87.28 85.62 85.82 85.04

III 86.99 91.91 86.38 86.32

R 4.59 12.47 1.61 1.28

I ² 61533.76 56796.42 64668.49 65946.24

II ² 68570.66 65971.92 66280.5 65091.32

III ²?68105.34 76021.52 67153.54 67060.28

K ² 198209.8 198789.9 198102.5 198097.8

S 39.77 233.13 4.02 2.46

Annotate: scutellarin content 0.390% in the medical material

Analysis of variance table

Factor S V MS F compares significance

A 39.77 2 19.89 16.17

B 233.13?2 116.57 94.77 *

C 4.02 2 2.01 1.63

D 2.46 2 1.23

By above-mentioned data as can be known, A2＞A3＞A1, B3＞B2＞B1, C3＞C2＞C1.B factor (extraction time) has the greatest impact to the rate of transform of scutellarin in the extract, and A factor (extraction time) is taken second place, and C factor (ethanol consumption) does not have influence.Intuitive analysis shows that under the condition of A3B3C2, the rate of transform of scutellarin is the highest, belongs to preferable condition.The results of analysis of variance shows: extraction time (B factor) has considerable influence should get B3 to the extraction ratio of scutellarin; There is certain influence extraction time (A factor) to the extraction ratio of scutellarin, but not remarkable, selects A2 in conjunction with orthogonal table; Ethanol consumption (C factor) does not have the significance influence to the extraction ratio of scutellarin, so select C1.Therefore determine that best extraction conditions is combined as A2B3C1.

2.1.3 Herba Erigerontis separation purifying technique condition research

Contain a large amount of impurity in the ethanol extraction, need further separation and purification.The prerun experimental result shows that polyamide column is to Herba Erigerontis scutellarin good separating effect, and in addition according to the dissolved character of flavones ingredient, we adopt the method for alkali extraction and acid precipitation that it is carried out further purification.

2.1.3.1 the preliminary remove impurity of extracting solution

Contain a large amount of impurity in the Herba Erigerontis ethanol extract,, make medicinal liquid obtain fine absorption, can avoid too much impurity to stop up chromatographic column simultaneously, influence separating effect so before extracting solution is with macroporous resin adsorption, will carry out preliminary remove impurity.

Method: take by weighing Herba Erigerontis medical material 900g, add 8 times of volume 70% ethanol, heating and refluxing extraction 3 times, each 1 hour.(60 ℃ of extracting solution decompression recycling ethanols,-0.09MPa), being concentrated into relative density is the concentrated solution of 1.03～1.05 (60 ℃), be divided into 3 parts behind the mix homogeneously, add not commensurability water for injection heating for dissolving, filter, precipitation and filtrate are dry respectively, investigate the influence of amount of water to scutellarin stripping situation.

Amount of water is to scutellarin stripping situation investigation table

Heavy (g) supernatant scutellarin content (%) the scutellarin rate of transform (%) of amount of water (ml) supernatant cream

600 10.76 8.51 78.26

900 11.42 8.75 85.41

1200 11.80 8.55 86.23

The result shows: when adding 900ml water for injection, precipitable most of impurity, can guarantee simultaneously the not too many loss of scutellarin again, can determine that thus the remove impurity condition is: extracting solution is concentrated into relative density at 1.03～1.05 (60 ℃), the water for injection heating for dissolving that adds 3 times of medical material volumes, filter, remove most of water-insoluble impurity.

2.1.3.2 the amount ratio of resin and Herba Erigerontis

The adsorption capacity of resin has certain limit, so the sample upper column quantity necessarily can not surpass its adsorption capacity, otherwise some compositions will run off.For avoiding producing this phenomenon, we measure the carrying capacity of AB-8 type macroporous resin adsorption Herba Erigerontis scutellarin.

Method: take by weighing the AB-8 macroporous resin 100g chromatographic column of packing into, the medicinal liquid that the remove impurity of learning from else's experience is handled makes medicinal liquid slowly pass through chromatographic column, up to the resin supersaturation, with water for injection resin is rinsed well, and is measured wherein Herba Erigerontis scutellarin weight, calculate carrying capacity by following formula:

Carrying capacity=(scutellarin amount in scutellarin upper column quantity-water lotion)/weight resin

AB-8 macroporous resin adsorption Herba Erigerontis carrying capacity investigation table

Scutellarin absorption scutellarin loading gage amount in the AB-8 macroporous resin scutellarin upper prop water lotion

Amount (g) is measured (g) (g) (g/100g) before the consumption

(g)

100 1.30 1.031 0.269 0.269

By the result as can be known: resin absorption Herba Erigerontis scutellarin carrying capacity is 0.269g scutellarin/100g resin, promptly is equivalent to 69g medical material/100g resin.In order to prevent the resin overload, reduce the loss of sample, each upper column quantity is decided to be 70% of carrying capacity, and promptly the per kilogram medical material needs 1.5 kilograms of resins.

2.1.3.3 elution requirement screening

In order to investigate the optimum condition of desorbing scutellarin from the resin column, select eluant strength, eluant consumption, the rate of outflow as the investigation factor, each factor is respectively got three levels, adopts L ₉(3 ⁴) orthogonal table tests.Get Herba Erigerontis medical material 1800g, add 8 times of volume 70% alcohol heating reflux and extract 3 times, each 1 hour, filter.Decompression filtrate recycling ethanol (60 ℃ ,-0.09MPa), being concentrated into relative density is the concentrated solution of 1.03～1.05 (60 ℃), adds the water for injection heating for dissolving of 3 times of medical material volumes behind the mix homogeneously, filter.Filtrate is divided into 9 parts (are every part and are equivalent to contain medical material 200g), crosses resin column post (interior diameter: post height=40mm: 400mm, weight resin 300g, volume 450ml).Begin to wash with the speed of 1L/kg medical material .h, press L then with the water for injection of 4 times of resin volumes and 15% ethanol of 4 times of resin volumes ₉(3 ⁴) orthogonal table carries out eluting, collects ethanol elution, decompression recycling ethanol, vacuum drying (60 ℃ ,-0.09Mpa).The rate of transform with scutellarin serves as to investigate index.

The factor level table

Factor flow velocity (L/kg medical material .h) concentration of alcohol (%) eluant consumption (doubly)

Horizontal A B C

1 8 40 3

2 10 50 4

3 12 60 5

Annotate: the eluant consumption is represented the weight resin multiple

The elution requirement orthogonal table

Gauge outfit

The A B C D scutellarin rate of transform (%)

Tested number

1 1 1 1 1 40.64

2 1 2 2 2 43.72

3 1 3 3 3 57.69

4 2 1 2 3 42.72

5 2 2 3 1 50.67

6 2 3 1 2 35.74

7 3 1 3 2 55.46

8 3 2 1 3 39.09

9 3 3 2 1 44.18

I 142.05 138.82 115.47 135.49

II 129.13 133.48 130.62 134.92

III 138.73 137.61 163.82 139.5

I ² 20178.2 19270.99?13333.32 18357.54

II ² 16674.56?17816.91?17061.58 18203.41

III ² 19246.01?18936.51?26836.99 19460.25

K ² 56098.77?56024.41?57231.9 56021.2

S 30.01 5.23 407.72 4.15

Eluting is analysis of variance table as a result

Soruces of variation S V F compares significance

A 30.01 2 7.23

B 5.23 2 1.26

C 407.72 2 98.25 *

D 4.15 2

By intuitive analysis as can be known, A3＞A2＞A1, B1＞B3＞B2, C3＞C2＞C1, solvent load (factor C) is the principal element that influences the scutellarin rate of transform, secondly is flow velocity (factor A) and concentration of alcohol (factor B).ANOVA showed significant: solvent load has the significance influence to the scutellarin rate of transform, selects best condition C 3; Concentration of alcohol does not have the significance influence to the scutellarin rate of transform, considers that the cost of factory selects B1; Flow velocity does not have the significance influence yet, selects condition A3 for use in order to shorten man-hour; So determine that elution requirement is A3B1C3, promptly be the speed eluting of 0.2ml/g medical material .min with 12L/kg medical material .h with 5 times of resin volume 40% ethanol.

2.2 Radix Ginseng Study on Preparation

2.2.1 the investigation of concentration of alcohol

According to the EXPERIMENTAL DESIGN of extraction process, Different concentrations of alcohol is carried out preferably.Design is respectively with 30%, 50% in the test, and 70%, 90% ethanol is as extracting solvent, serves as to investigate index with the rate of transform of total saponins in the extract, and different extraction solvents is investigated.

Test method: take by weighing 4 parts of Radix Ginsengs, every part of 200g adds the different solvents of 10 times of volumes, reflux, extract, 3 times, each 1 hour respectively.Respectively extracting solution is filtered, decompression filtrate recycling ethanol (60 ℃) concentrates, vacuum drying (60 ℃ ,-0.09Mpa).Measure the content of Radix Ginseng total saponins.

The investigation table of concentration of alcohol

Heavy (g) total saponin content (%) rate of transform (%) of concentration of alcohol (%) medical material weight (g) cream

30 200.01 32.95 4.23 79.19

50 200.05 32.17 4.44 81.16

70 200.03 25.70 6.28 90.24

90 200.03 23.37 6.14 89.50

Annotate: Radix Ginseng total saponins content 0.88% in the medical material

The result shows, during with 70% ethanol extraction, the total saponin content and the rate of transform all are higher than the ethanol of other concentration.So the ethanol of selection 70% is as extracting solvent.

2.2.2 the optimization of extraction conditions

Main active site in the Radix Ginseng is a saponin component, such constitutive property is more stable, and therefore good heat resistance adopts ethanol refluxing process to extract, and the principal element that influences the reflux, extract, effect has: solvent load, extraction time and extraction time, therefore these major influence factors are investigated.As investigating index, adopt L with the rate of transform of Radix Ginseng total saponins ₉(3 ⁴) the preferred extraction conditions of orthogonal test.

Experimental technique and data

Take by weighing Radix Ginseng 300g, totally 9 parts, make solvent with 70% ethanol, respectively by orthogonal table L ₉(3 ⁴) test.

Radix Ginseng extracts the experimental factor water-glass

Factor level A extraction time (h) B extraction time (inferior) C solvent load (doubly)

1 1 1 8

2 1.5 2 10

3 2 3 12

Radix Ginseng extracts orthogonal test table

Factor

The A B C D rate of transform (%)

Level

1 1 1 1 1 74.26

2 1 2 2 2 90.24

3 1 3 3 3 91.51

4 2 1 2 3 77.47

5 2 2 3 1 89.69

6 2 3 1 2 88.78

7 3 1 3 2 81.13

8 3 2 1 3 87.01

9 3 3 2 1 92.16

I 256.01 232.86 250.05 256.11

II 255.94 266.94 259.87 260.15

III_ 260.30 272.45 262.33 255.99

I_ 85.34 77.62 83.35 85.37

II_ 85.31 88.98 86.62 86.72

III 86.77 90.82 87.44 85.33

R 1.45 13.20 4.09 1.39

I ² 65541.12 54223.78 62525.00 65592.33

II ² 65505.28 71256.96 67532.42 67678.02

III ² 67756.09 74229.00 68817.03 65530.88

K ² 198802.49?199709.75?198874.45?198801.23

S 4.16 306.57 28.14 3.74

Annotate: total saponin content 0.88% among the ginseng crude drug

Analysis of variance table

Soruces of variation sum of deviation square degree of freedom variance F value

A 4.16 2 2.08 1.11

B 306.57 2 153.29 81.97

C 28.14 2 14.07 7.52

D 3.74 2 1.87

By The above results as can be known, A2＞A1＞A3, B3＞B2＞B1, C3＞C2＞C1.B factor (extraction time) is bigger to the rate of transform influence of total saponins in the extract, the no significance influence of A factor and C factor (solvent load).Intuitive analysis shows that under the condition of A3B3C2, the rate of transform of total saponins is the highest, belongs to preferable condition; The results of analysis of variance shows: extraction time (B factor) has considerable influence should get B3 to the rate of transform of total saponins; Extraction time (A factor) does not have obvious influence to the rate of transform of total saponins, selects A1 in conjunction with the data in the orthogonal table; Solvent load (C factor) does not have the significance influence to the rate of transform of total saponins, so select C1.Therefore determine that extraction conditions is A1B3C1, promptly measure 70% ethanol, reflux, extract, 3 times, each 1 hour for 8 times.

2.2.3 the separation and purification condition is investigated

At present the more satisfactory method of separation and purification Radix Ginseng total saponins is the method for macroporous resin column chromatography, so we select for use the more satisfactory ZTC-1 type resin of separating effect to come the purification Radix Ginseng total saponins, and its separation condition is investigated.

In order to investigate the optimum condition of desorbing total saponins from the resin, select eluant strength, eluant consumption, three factors of effluent speed, each factor is respectively got three levels, adopts L ₉(3 ⁴) orthogonal table tests, get ginseng crude drug 2700g, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 4 times of medical material volumes, filter, filtrate is divided into 9 parts of speed with 0.5ml/g medical material .min and crosses ZTC-1 type macroporous adsorbent resin, uses 7 times of resinite hydrops and 5 times of resin volume 10% alcohol flushing impurity successively, carries out eluting with alcoholic solution then, collect ethanol elution, be concentrated into dried.With must measuring of total saponins is index.

C effluent speed

Factor

A concentration of alcohol (%) B eluant consumption (doubly) (ml/g medicine

Level

Material .min)

1 20 5 0.6

2 40 7 0.8

3 60 9 1.0

Experimental result

Gauge outfit

A B C D total saponins amount (g)

Tested number

1 1 1 1 1 2.07

2 1 2 2 2 2.09

3 1 3 3 3 2.11

4 2 1 2 3 2.97

5 2 2 3 1 3.07

6 2 3 1 2 3.40

7 3 1 3 2 3.30

8 3 2 1 3 3.56

9 3 3 2 1 3.97

I 6.27 8.34 9.03 9.11

II 9.44 8.72 9.03 8.79

III 10.83 9.48 8.48 8.64

I 2.09 2.78 3.01 3.04

II 3.15 2.91 3.01 2.93

III 3.61 3.16 2.83 2.88

R 1.52 0.38 0.18 0.16

I ² 39.31 69.56 81.54 82.99

II ² 89.11 76.04 81.54 77.26

III ²?117.29 89.87 71.91 74.65

K ² 245.71 235.47 234.99 234.90

S 3.64 0.23 0.07 0.04

The separation condition analysis of variance table

Soruces of variation SS V MS F compares significance

A 3.64 2 1.82 91 *

B 0.23 2 0.12 6

C 0.07 2 0.04 2

D 0.04 2 0.02

Look into F show F _(1-0.05)(2,2)=19, F _(1-0.01)(2,2)=99,

By intuitive analysis as can be known, A ₃＞A ₂＞A ₁, B ₃＞B ₂＞B ₁, C ₁=C ₂＞C ₃, elution volume (factor A) has certain influence to the separation of total saponins, and concentration of alcohol (factor B) and flow velocity (factor C) influence are little.ANOVA showed significant, elution volume has appreciable impact to the separation of total saponins, selects best condition A ₃, concentration of alcohol does not have influence, considers that the cost of factory selects B ₁, flow velocity does not have influence, selects condition C for use in order to shorten man-hour ₃So, determine the A that is combined as of elution requirement ₃B ₁C ₃, promptly with 5 times of column volume 60% ethanol with 1ml/g medical material .min speed eluting.(with A ₃B ₁C ₃Corresponding)

2.3 Radix Ophiopogonis Study on Preparation

2.3.1 Radix Ophiopogonis, the water extraction condition was investigated

2.3.1.1 water absorption rate is investigated

Medical material is a dry product when decocting for the first time, and itself will absorb moisture, and for preventing the influence of medical material suction to amount of water, the spy makes water absorption rate and investigates, and adds corresponding water absorption when decocting for the first time.

Get 200g medical material Radix Ophiopogonis during investigation and add 10 times of water gagings, be dipped to the heart, filter, recording water absorption rate is 240%.

2.3.1.2 factor level is selected

The Chinese medicine preparation curative effect depends primarily on extraction, and extraction effect is subjected to extracting the influence of factors such as solvent, extraction time and time.Main active component is polysaccharide and saponins in Radix Ophiopogonis, and the two all has fine solubility in water, therefore takes into account both extractions, and preliminary definite extraction solvent is a water.The general investigation decocts when extracting, and chooses amount of water, decocting time, decoction number of times as factor, and the varying level of each factor of high spot reviews is to decocting the influence of extraction effect.According to knowhow and practical situation, the selection factor level.

Extract the experimental factor water-glass Radix Ophiopogonis

Factor level A amount of water (doubly) B decocts number of times (inferior) C decocting time (h)

1 6 1 1

2 8 2 1.5

3 10 3 2

Extract orthogonal test table Radix Ophiopogonis

Factor

The A B C D rate of transform (%)

Level

1 1 1 1 1 73.62

2 1 2 2 2 80.14

3 1 3 3 3 88.51

4 2 1 2 3 80.47

5 2 2 3 1 86.26

6 2 3 1 2 90.87

7 3 1 3 2 79.31

8 3 2 1 3 85.17

9 3 3 2 1 92.16

I 242.27 233.40 249.66 252.0

II 257.60 251.57 252.77 250.32

III 256.64 271.54 254.08 254.15

I 80.76 77.80 83.22 84.01

II 85.87 83.86 84.26 83.44

III 85.55 90.51 84.69 84.72

R 5.11 12.71 1.47 1.28

I ² 58694.75 54475.56 62330.12 63524.16

II ² 66357.76 63287.46 63892.67 62660.10

III ²?65864.09 73733.97 64556.65 64592.22

K ² 190916.60 191497.00 190779.43 190776.49

S 49.16 242.62 3.44 2.45

Annotate: total polysaccharides content 8.55% in the Radix Ophiopogonis medical material

Analysis of variance table

Soruces of variation sum of deviation square degree of freedom variance F value

A 49.16 2 24.58 19.98

B 242.62 2 121.31?98.63

C 3.44 2 1.72 1.40

D 2.45 2 1.23

By The above results as can be known, A2＞A3＞A1, B3＞B2＞B1, C3＞C2＞C1.B factor (amount of water) is bigger to the rate of transform influence of total polysaccharides in the extract, and A factor (solvent load) has certain influence but is not clearly, the no significance influence of C factor (extraction time).Intuitive analysis shows that under the condition of A3B3C2, the rate of transform of total polysaccharides is the highest, belongs to preferable condition; The results of analysis of variance shows: amount of water (B factor) has considerable influence should get B3 to the rate of transform of total polysaccharides; Extraction time (A factor) has certain influence to the rate of transform of total polysaccharides, selects A2 in conjunction with the data in the orthogonal table; Extraction time (C factor) does not have the significance influence to the rate of transform of total polysaccharides, so select C1.Therefore determine that extraction conditions is A2B3C1, promptly 8 times of water gagings extract each 1 hour 3 times.

2.3.1.3 saponin separation condition screening test

Get medical material 2700g Radix Ophiopogonis, adding 8 times of volume decoctings boils 3 times, each 1 hour, merge extractive liquid, filtered, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.5ml/g medical material .min, water with 6 times of resin volumes washes with the speed of 1ml/g medical material .min earlier, sample effluent and water lotion in the collection, and measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 60%, make that to contain the alcohol amount be 85% for the second time, filter, twice precipitation merged the back add 2 times of water dissolutioies, filter, measuring relative density when filtrate decompression is concentrated into 60 ℃ is 1.05～1.15, gets Radix Ophiopogonis polysaccharide, 20% ethanol of 3 times of resin volumes of reuse is with the speed eluting impurity of 1ml/g medical material .min, use the alcoholic solution eluting at last, collect stripping liquid, concentrate drying, measure total saponin content, calculate the rate of transform.

The factor level table

Factor A effluent speed (ml/g

B eluant consumption (doubly) C concentration of alcohol (%)

Horizontal medical material .min)

1 0.4 4 40

2 0.6 6 50

3 0.8 8 60

Orthogonal table

The factor rate of transform

A B C D

Experiment number (%)

1 1 1 1 1 37.66

2 1 2 2 2 52.05

3 1 3 3 3 54.73

4 2 1 2 3 45.74

5 2 2 3 1 61.3

6 2 3 1 2 44.32

7 3 1 3 2 51.66

8 3 2 1 3 41.57

9 3 3 2 1 44.14

I 144.44 135.06 123.55 143.1

II 151.36 154.92 141.93 148.03

III 137.37 143.19 167.69 142.04

I ² 20862.91 18241.20 15264.60 20477.61

II ² 22909.85 24000.21 20144.12 21912.88

III ² 18870.52 20503.38 28119.94 20175.36

K ² 62643.28 62744.79 63528.66 62565.85

S 32.62 66.46 327.75 6.81

Analysis of variance table

The mean square F ratio of soruces of variation sum of deviation square degree of freedom

A 32.62 2 16.31 4.79

B 66.46 2 33.23 9.76

C 327.75 2 163.87?48.11

D 6.81 2 3.41

From above-mentioned variance analysis and orthogonal table as can be seen, the concentration of alcohol influence is bigger, gets 60% alcohol desorption; Volume and flow velocity do not have influence, consider production cost and working time, select 4 times of volumes and 0.8ml/g medical material .min respectively for use.

Experimental example 3: injection with small volume or concentrated solution for injection molding research

3.1 activated carbon dosage is investigated:

Injection owing to solvent, raw material, container etc. have the pyrogen material, reduces the safety of injection in the process of producing, and therefore needs to remove the pyrogen material in the process of preparation injection.The method of depyrogenation mainly contains high temperature method, acid-base method, ultrafiltration and absorption method at present, active carbon adsorption not only can heat of adsorption originality composition, the effect that also has filter of helping and decolouring, when removing pyrogen, can improve the appearance character of preparation, therefore we select the active carbon adsorption depyrogenation for use, and its consumption investigated, the results are shown in following table:

The activated carbon dosage investigation table

Heavy (g) rate of transform (%) outward appearance of activated carbon dosage (%) cream

0.1 6.45 54.67 is reddish brown

1 6.31 53.84 is red

1.5 6.17 51.15 is red

From the medicinal liquid outward appearance, select activated carbon dosage be 1% and 1.5% proper; But judge that from the rate of transform 0.1% consumption and 1% consumption are slightly better, the three all can satisfy the related request of injection, but takes all factors into consideration above factor, so that be the best with the activated carbon decolorizing of medicine liquid volume 1%.

The bleaching time investigation table

Time (minute) heavy (g) rate of transform (%) outward appearance of cream

10 6.72 53.20 is reddish brown

30 6.35 52.69 is red

60 6.03 49.72 is pale red

From top test as can be seen, along with the color of the prolongation medicinal liquid of time is thin out, but above-mentioned factor is taken all factors into consideration in the also corresponding minimizing of the rate of transform of effective ingredient, selects for use and boils 30 minutes for best.

3.2 pH value of solution is investigated

For adapting to the Human Physiology needs, also to consider the character of each constituents in the medicinal liquid simultaneously, when dosing, need suitably adjust the pH value of medicinal liquid.Select scutellarin content as evaluation index.

Test method and result: after feeding intake and handle by recipe quantity,, filter with the concentrated solution mix homogeneously by above-mentioned condition, add water to 1000ml, adjust pH is when the different pH value that reaches shown in the following table, boil the back standing over night, observe the variation of appearance character under different pH condition.Experimental result sees Table:

The investigation of dosing pH value

Sequence number 123456789

Dosing pH 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5

Boil pH 4.0 4.4 5.1 5.7 6.2 6.6 7.1 7.7 8.3

The no significant change color burn of precipitation appears in outward appearance

The result shows, the medicinal liquid pH value boils the back at the sample below 5.5 and precipitation occurs, and pH value is obviously deepened in the color sample more than 7.5, and pH value is that 5.5～7.5 medicinal liquid is relatively stable, and outward appearance does not have significant change.Below its scutellarin content is measured.The results are shown in Table:

The situation of change table of index components before and after pH value is regulated

Content (%) boils back pH and boils back content (%) during sequence number dosing pH dosing

1 5.5 5.17 5.1 4.89

2 6.0 5.17 5.7 5.06

3 6.5 5.17 6.2 4.93

4 7.0 5.17 6.6 5.10

5 7.5 5.17 7.1 5.09

As seen from table, medicinal liquid is being adjusted the pH value front and back, the not too big variation of index components scutellarin content.The appearance character of comprehensive above-mentioned medicinal liquid and the changes of contents of scutellarin, the pH value of medicinal liquid is transferred between 5.5～7.5 when determining dosing.

Experimental example 4: the investigation of lyophilized formulations moulding process

4.1 the screening of caffolding agent kind

The caffolding agent kind influences the molding of freeze-dried powder, so at first this is screened.Taking liquid mixes with caffolding agent mannitol, glucose and lactose solution respectively, 0.22 μ m membrane filtration postlyophilization, every XiLin bottle-packaging solution 3ml.Freeze dryer: Edwards SNL-3200 freezer dryer (the thermoelectric Thermo of the U.S.).Lyophilisation condition :-45 ℃, behind the pre-freeze 8h, the beginning evacuation, and be warming up to-40 ℃, keep 10h; Be warming up to-30 ℃, keep 10h; Be warming up to-20 ℃, keep 10h; Be warming up to-10 ℃, keep 5h; Be warming up to 0 ℃, keep 5h; Be warming up to 15 ℃, keep 3h; Be warming up to 25 ℃, keep 3h, the result is as showing:

The screening of caffolding agent kind

Caffolding agent kind caffolding agent: medicinal liquid (V: V) solubility finished product outward appearance

5: 4 good parts of glucose subside

Galactose general molding in 5: 4

Mannitol good molding in 5: 4

Glycine good molding in 5: 4, frangible

Dextran general molding in 5: 4

Mannitol, propylene glycol good molding in 5: 4

Glycine, Polyethylene Glycol good molding in 5: 4, frangible

Dextran, sorbitol, tween good molding in 5: 4

Blank medicinal liquid 3ml atrophy

As seen from table, in the adjuvant that is screened, under the identical situation of other conditions, most of adjuvant all can be made into freeze-dried powder, but solubility angle integrated survey from yield rate, molding situation and sample, use the effect of mannitol to be better than other several adjuvants separately, can satisfy the every requirement of injection, reduce simultaneously as far as possible and add too much adjuvant.

4.2 caffolding agent consumption screening

The mannitol solution (40mg/ml, 100mg/ml and 160mg/ml) of variable concentrations is mixed in varing proportions with medicinal liquid, filter, every cillin bottle loading amount is 3ml, lyophilization.Lyophilisation condition :-45 ℃, behind the pre-freeze 8h, the beginning evacuation, and be warming up to-40 ℃, keep 10h; Be warming up to-30 ℃, keep 10h; Be warming up to-20 ℃, keep 10h; Be warming up to-10 ℃, keep 5h; Be warming up to 0 ℃, keep 5h; Be warming up to 15 ℃, keep 3h; Be warming up to 25 ℃, keep 3h.The result is as showing:

The screening of mannitol consumption

Mannitol concentration mannitol: medicinal liquid

Numbering color and luster profile solubility clarity

(mg/ml) (v∶v)

1 40 5: 4 yellowish-brown parts have been subsided up to specification

2 100 5: 4 is yellow intact good up to specification

3 160 5: 4 is yellowish intact good up to specification

As seen from table, when the ratio of caffolding agent consumption and medicinal liquid is 5: 4, the sample character is that the sample of 100mg/ml and 160mg/ml is relatively good with the mannitol concentration, the sample of 40mg/ml has part to subside, but major part still is molding, but take all factors into consideration the consumption and the clinical dose of adjuvant, the optimum selection mannitol concentration is 100mg/ml, and the volume ratio of mannitol solution and medicinal liquid is 5: 4.

4.3 lyophilization conditional filtering

Lyophilization is a veryer long dry run, needs to consume a large amount of energy.An ideal lyophilisation condition not only can be saved a large amount of energy, can also shorten man-hour simultaneously, so we are optimized screening to existing lyophilisation condition.The actual conditions screening sees Table:

The lyophilization conditional filtering

Time (h)

Condition I condition II condition III cold-trap

Temperature (℃)

-45 (pre-freezes) 10-8

-40 (pre-freeze)-8-

-40 (evacuation) 8-10

-35 (evacuation)-8-

-30 (evacuation) 8-9 keeps

-25 (evacuation)-9--70 ℃

-20 (evacuation) 8-10

-15 (evacuation)-8-

-10 (evacuation) 6-5

0 (evacuation) 554

10 (evacuation) 243

20 (evacuation) 243

Experimental result shows: finished product appearance character that condition I, II and III make and the equal conformance with standard of moisture.But comparatively speaking, condition II yield rate is low slightly, and condition III power consumption is bigger, considers the practical situation of production, short condition I of finally selected overall time spent, i.e. and lyophilization condition is: pre-freeze temperature-45 ℃, pre-freeze time 10h;-40 ℃ of evacuation keep 8h; Be warming up to-30 ℃ again, keep 8h; Be warming up to-20 ℃, keep 8h; Be warming up to-10 ℃, keep 6h; Be warming up to 0 ℃, keep 5h; Be warming up to 10 ℃, keep 2h; Be warming up to 20 ℃, keep 2h, get product.

Experimental example 5: spray drying conditional filtering

Spray drying technology can make sample dry rapidly under the situation of atomizing, and the protection effective ingredient can make the water content of sample reduce simultaneously, helps stability of formulation.It is bigger that but the air temperature and current speed that spray-dired effect is imported and exported influences, so we are that evaluation index is investigated these three factors with the loss of active ingredients rate.

Spray drying condition investigation table

Inlet temperature (℃) outlet temperature (℃) air velocity (ms ^-1) loss rate (%)

140 60 16 3.76

150 70 18 2.93

160 80 20 3.30

From above-mentioned result of the test as can be seen, three kinds of conditions all can obtain material preferably, but are 150 ℃ with inlet temperature by contrast, and outlet temperature is 70 ℃, and air velocity is 18ms ^-1Condition be best.

Concrete embodiment

(part is represented weight portion, as: kilogram, gram etc.)

Embodiments of the invention 1: 300 parts of 125 parts of Herba Erigerontiss of 125 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 0.1% active carbon, boil, keep little 10min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, adjust pH 5.5 boiled, 1 ℃ of cold preservation 12 hours, coarse filtration, fine straining, dividing to install in the ampoule bottle, is 100 ℃ in vapor (steam) temperature, and actual pressure is at 100kN/m ³Pressure sterilizing is 40 minutes under the condition, promptly gets the injection with small volume or the concentrated solution for injection that are directly used in drug administration by injection.After testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 27% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 19% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 17% of total solid after deduction adjuvant amount and the water quantities; The total solid that three's sum accounts in the preparation after deduction adjuvant amount and the water quantities is 63%.

Embodiments of the invention 2: 300 parts of 125 parts of Herba Erigerontiss of 125 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, add the glucose of ormal weight again, by volume add 1.5% active carbon, boil, keep little 60min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, adjust pH 7.5, boil, at 8 ℃ of cold preservations 12 hours, coarse filtration, fine straining, add the injection water, packing is under 125 ℃ of conditions, sterilized 60 minutes, and promptly got the glucose intravenous infusion agent.After testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 36% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 17% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 17% of total solid after deduction adjuvant amount and the water quantities; The total solid that three's sum accounts in the preparation after deduction adjuvant amount and the water quantities is 70%.

Embodiments of the invention 3: 300 parts of 125 parts of Herba Erigerontiss of 125 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, add the sodium chloride of ormal weight again, by volume add 0.1% active carbon, boil, keep little 10min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, transfer pH value 5.5, boil, at 1 ℃ of cold preservation 12 hours, coarse filtration, fine straining, add the injection water, packing is under 105 ℃ of conditions, sterilized 20 minutes, and promptly got the sodium chloride intravenous infusion agent.

Embodiments of the invention 4: 300 parts of 125 parts of Herba Erigerontiss of 125 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 1.5% active carbon, boil, keep little 60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 7.5, boil, 8 ℃ of cold preservations 12 hours, coarse filtration, fine straining divide to install in the enamel tray, temperature-45 ℃, pre-freeze time 12h, the beginning evacuation, and be warming up to-37 ℃, keep 10h, be warming up to-27 ℃ again, keep 10h; Be warming up to-17 ℃, keep 10h, be warming up to-7 ℃, keep 6h, be warming up to 3 ℃, keep 6h, be warming up to 13 ℃, keep 3h, be warming up to 23 ℃, keep 3h, under aseptic condition, divide to install to promptly to get the freeze dry sterile powder end in the cillin bottle.

Contain saponin component, polysaccharide composition and flavones ingredient in the preparation, calculate according to percentage by weight, wherein the content of saponin component accounts for the total solid 1% after the deduction adjuvant amount and water quantities in the preparation; The content of flavones ingredient accounts in the preparation total solid 1% after deduction adjuvant amount and the water quantities, and the content of polysaccharide composition accounts for 3% of the total solid after the deduction adjuvant amount and water quantities in the preparation.

Embodiments of the invention 5: 300 parts of 125 parts of Herba Erigerontiss of 125 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 0.1% active carbon, boil, keep little 10min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, adjust pH 5.5 boiled, 1 ℃ of cold preservation 12 hours, coarse filtration, fine straining, in inlet temperature is 140 ℃, and leaving air temp is 60 ℃, and air velocity is 16ms ^-1Condition under spray drying get powder, packing promptly gets the spray drying sterilized powder.After testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 41% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 13% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 19% of total solid after deduction adjuvant amount and the water quantities; The total solid that three's sum accounts in the preparation after deduction adjuvant amount and the water quantities is 73%.

Embodiments of the invention 6: 5000 parts of 1000 parts of Herba Erigerontiss of 1000 parts of Radix Ginsengs Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 15 times of volume decoctings boils 4 times, each 2.5 hours, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.8ml/g medical material .min, water with 10 times of resin volumes washes with the speed of 1.5ml/g medical material .min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 70%, make for the second time that to contain the alcohol amount be 90%, filter, will twice precipitation merge the back and add 2 times of water dissolutioies, filter, filtrate concentrate Radix Ophiopogonis polysaccharide, 25% ethanol of 4 times of resin volumes of reuse is used the speed eluting of 70% ethanol of 6 times of resin volumes with 1.0ml/g medical material .min at last with the speed eluting impurity of 1.5ml/g medical material .min, collect stripping liquid, merge with above-mentioned Radix Ophiopogonis polysaccharide after reclaiming ethanol, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 15 times of volume 80% alcohol reflux 4 times, each 2.5 hours, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 5 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.8ml/g medical material .min, use 10 times of resinite hydrops and 6 times of resin volume 15% alcohol flushing impurity successively, use 70% alcohol desorption of 7 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the ginseng crude drug, add 15 times of volume 80% alcohol reflux 4 times, each 2.5 hours, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 5 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 1.5ml/g medical material .min, use 10 times of resinite hydrops and 6 times of resin volume 15% alcohol flushing impurity successively, use 70% alcohol desorption of 7 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

The said extracted thing is merged, add an amount of water for injection dissolving, by volume add 1% active carbon, boil, keep little 30min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfers pH value 7.5, boils, at 4 ℃ of cold preservations 12 hours, coarse filtration, fine straining.Mannitol is added the injection water be mixed with 100mg/ml solution,, filter, packing, temperature-45 ℃, pre-freeze time 10h with above-mentioned filtrate mixing;-40 ℃ of evacuation keep 8h; Be warming up to-30 ℃ again, keep 8h; Be warming up to-20 ℃, keep 8h; Be warming up to-10 ℃, keep 6h; Be warming up to 0 ℃, keep 5h; Be warming up to 10 ℃, keep 2h; Be warming up to 20 ℃, keep 2h, promptly get freeze-dried powder.After testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 47% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 22% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 21% of total solid after deduction adjuvant amount and the water quantities; The total solid that three's sum accounts in the preparation after deduction adjuvant amount and the water quantities is 90%.

Embodiments of the invention 7: 50 parts of 10 parts of Herba Erigerontiss of 10 parts of Radix Ginsengs Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 5 times of volume decoctings boiled 1 time 0.5 hour, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.3ml/g medical material .min, water with 3 times of resin volumes washes with the speed of 0.5ml/g medical material .min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add ethanol precipitate with ethanol twice, make that to contain the alcohol amount be 50% for the first time, make that to contain the alcohol amount be 80% for the second time, filter, will twice precipitation merge the back and add 1 times of water dissolution, filter, filtrate concentrate Radix Ophiopogonis polysaccharide, 5% ethanol of 1 times of resin volume of reuse is with the speed eluting impurity of 0.5ml/g medical material .min, use the speed eluting of 50% ethanol of 2 times of resin volumes at last, collect stripping liquid, merge with above-mentioned Radix Ophiopogonis polysaccharide behind the recovery ethanol with 0.5ml/g medical material .min, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, added 5 times of volumes, 50% alcohol reflux 1 time 0.5 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 1 times of medical material volume, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.1ml/g medical material .min, use 1 times of resinite hydrops and 1 times of resin volume 5% alcohol flushing impurity successively, use 30% alcohol desorption of 1 times of resin volume then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the ginseng crude drug, added 5 times of volumes, 50% alcohol reflux 1 time 0.5 hour, measuring relative density during extracting solution decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 1 times of medical material volume, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 0.3ml/g medical material .min, use 1 times of resinite hydrops and 1 times of resin volume 5% alcohol flushing impurity successively, use 30% alcohol desorption of 1 times of resin volume then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

The said extracted thing is merged, add an amount of water for injection dissolving, by volume add 0.1% active carbon, boil, keep little 60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 5.5, boil, 8 ℃ of cold preservations 12 hours, coarse filtration, fine straining, dividing to install in the ampoule bottle, is 110 ℃ in vapor (steam) temperature, and actual pressure is at 120kN/m ³Pressure sterilizing is 60 minutes under the condition, promptly gets the injection with small volume or the concentrated solution for injection that are directly used in drug administration by injection.After testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 21% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 3% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 1% of total solid after deduction adjuvant amount and the water quantities; The total solid that three's sum accounts in the preparation after deduction adjuvant amount and the water quantities is 25%.

Embodiments of the invention 8: 300 parts of 60 parts of Herba Erigerontiss of 110 parts of Radix Ginsengs Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 15 times of volume decoctings boils 4 times, each 2.5 hours, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.8ml/g medical material .min, water with 10 times of resin volumes washes with the speed of 1.5ml/g medical material .min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 70%, make for the second time that to contain the alcohol amount be 90%, filter, will twice precipitation merge the back and add 4 times of water dissolutioies, filter, filtrate concentrate Radix Ophiopogonis polysaccharide, 15% ethanol of 3 times of resin volumes of reuse is used the speed eluting of 60% ethanol of 5 times of resin volumes with 0.8ml/g medical material .min at last with the speed eluting impurity of 1ml/g medical material .min, collect stripping liquid, merge with above-mentioned Radix Ophiopogonis polysaccharide after reclaiming ethanol, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, added 5 times of volumes, 50% alcohol reflux 1 time 0.5 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 1 times of medical material volume, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.3ml/g medical material .min, use 1 times of resinite hydrops and 1 times of resin volume 5% alcohol flushing impurity successively, use 30% alcohol desorption of 1 times of resin volume then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

The said extracted thing is merged, add an amount of water for injection dissolving, add the glucose of ormal weight again, by volume add 0.1% active carbon, boil, keep little 10min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, transfer pH value 7.5, boil, at 1 ℃ of cold preservation 12 hours, coarse filtration, fine straining, add the injection water, packing is under 105 ℃ of conditions, sterilized 20 minutes, and promptly got the glucose intravenous infusion agent.After testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 50% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 1% of total solid after deduction adjuvant amount and the water quantities.

Embodiments of the invention 9: 400 parts of 100 parts of Herba Erigerontiss of 100 parts of Radix Ginsengs Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 10 times of volume decoctings boils 3 times, each 1.5 hours, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.5ml/g medical material .min, water with 6 times of resin volumes washes with the speed of 1ml/g medical material .min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 60%, make for the second time that to contain the alcohol amount be 85%, filter, will twice precipitation merge the back and add 2 times of water dissolutioies, filter, measuring relative density when filtrate decompression is concentrated into 60 ℃ is 1.05～1.15, gets Radix Ophiopogonis polysaccharide, and 20% ethanol of 3 times of resin volumes of reuse is with the speed eluting impurity of 1ml/g medical material .min, use the speed eluting of 60% ethanol of 4 times of resin volumes at last with 0.8ml/g medical material .min, collect stripping liquid, merge with above-mentioned Radix Ophiopogonis polysaccharide behind the recovery ethanol, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 3 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.5ml/g medical material .min, use 5 times of resinite hydrops and 4 times of resin volume 10% alcohol flushing impurity successively, use 40% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the ginseng crude drug, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 4 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 0.5ml/g medical material .min, use 7 times of resinite hydrops and 5 times of resin volume 10% alcohol flushing impurity successively, use 60% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

The said extracted thing is merged, add an amount of water for injection dissolving, add the sodium chloride of ormal weight again, by volume add 1% active carbon, boil, keep little 30min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, transfer pH value 5.5, boil, at 4 ℃ of cold preservations 12 hours, coarse filtration, fine straining, add the injection water, packing is under 115 ℃ of conditions, sterilized 30 minutes, and promptly got the sodium chloride intravenous infusion agent.After testing, contain saponin component 50% in the effective site Radix Ginseng total saponins of Radix Ginseng, contain saponin component 50% in the effective site Radix Ophiopogonis total saponins of Radix Ophiopogonis, contain polysaccharide composition 50% in the another one effective site Radix Ophiopogonis polysaccharide of Radix Ophiopogonis, contain flavones ingredient 50% in the effective site Herba Erigerontis total flavones of Herba Erigerontis.

Embodiments of the invention 10: 500 parts of 100 parts of Herba Erigerontiss of 150 parts of Radix Ginsengs Radix Ophiopogonis

A, add 10 times of volumes, 70% alcohol reflux Radix Ophiopogonis 3 times, each 1 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, filter merging filtrate, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, medicinal residues add 5 times of volume decoctings and boil 2 times, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, merge above-mentioned concentrated solution, add the dissolving of 6 times of amount water for injection, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.6ml/g medical material .min, water with 5 times of resin volumes washes with the speed of 0.6ml/g medical material .min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 60%, make for the second time that to contain the alcohol amount be 85%, filter, will twice precipitation merge the back and add 3 times of water dissolutioies, filter, filtrate concentrate Radix Ophiopogonis polysaccharide, 10% ethanol of 3 times of resin volumes of reuse is with the speed eluting impurity of 1ml/g medical material .min, use the speed eluting of 60% ethanol of 6 times of resin volumes at last, collect stripping liquid, merge with above-mentioned Radix Ophiopogonis polysaccharide behind the recovery ethanol with 0.8ml/g medical material .min, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

C, get the ginseng crude drug, adding 12 times of volume decoctings boils 3 times, each 1.5 hours, merge extractive liquid,, cross ZTC-1 type macroporous adsorbent resin with the speed of 0.5ml/g medical material .min, with 6 times of resinite hydrops flushings, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 50%, make that to contain the alcohol amount be 80% for the second time, filter, twice precipitation merged the back add 2 times of water dissolutioies, filter, filtrate concentrate the ginseng polysaccharide, 4 times of resin volumes of reuse, 10% alcohol flushing impurity, use 50% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

The said extracted thing is merged, add an amount of water for injection dissolving, by volume add 0.1%～1.5% active carbon, boil, keep little 10～60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 7.5, boil, 1～8 ℃ of cold preservation 12 hours, coarse filtration, fine straining, divide to install in the enamel tray temperature-45 ℃, pre-freeze time 10h;-40 ℃ of evacuation keep 8h; Be warming up to-30 ℃ again, keep 8h; Be warming up to-20 ℃, keep 8h; Be warming up to-10 ℃, keep 6h; Be warming up to 0 ℃, keep 5h; Be warming up to 10 ℃, keep 2h; Be warming up to 20 ℃, keep 2h, under aseptic condition, divide to install to promptly to get the freeze dry sterile powder end in the cillin bottle.

Embodiments of the invention 11: 1000 parts of 200 parts of Herba Erigerontiss of 200 parts of Radix Codonopsis Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 8 times of volume decoctings boils 3 times, each 1.5 hours, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.4ml/g medical material .min, water with 6 times of resin volumes washes with the speed of 0.7ml/g medical material .min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 65%, make for the second time that to contain the alcohol amount be 80%, filter, will twice precipitation merge the back and add 3 times of water dissolutioies, filter, filtrate concentrate Radix Ophiopogonis polysaccharide, 15% ethanol of 4 times of resin volumes of reuse is used the speed eluting of 70% ethanol of 4 times of resin volumes with 0.8ml/g medical material .min at last with the speed eluting impurity of 1.2ml/g medical material .min, collect stripping liquid, merge with above-mentioned Radix Ophiopogonis polysaccharide after reclaiming ethanol, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 12 times of volume 60% alcohol reflux 2 times, each 0.8 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 4 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.6ml/g medical material .min, use 4 times of resinite hydrops and 5 times of resin volume 8% alcohol flushing impurity successively, use 50% alcohol desorption of 7 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get codonopsis pilosula, add 10 times of volume 70% alcohol reflux 2 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 4 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 0.5ml/g medical material .min, use 7 times of resinite hydrops and 5 times of resin volume 10% alcohol flushing impurity successively, use 60% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Codonopsis extract;

The said extracted thing is merged, add an amount of water for injection dissolving, by volume add 0.8% active carbon, boil, keep little 40min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 5.5～7.5, boil, 6 ℃ of cold preservations 12 hours, coarse filtration, fine straining, in inlet temperature is 150 ℃, and leaving air temp is 70 ℃, and air velocity is 18ms ^-1Condition under spray drying get powder, packing promptly gets the spray drying sterilized powder.

Embodiments of the invention 12: 100 parts of 10 parts of Herba Erigerontiss of 10 parts of Radix Ginsengs Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 5 times of volume decoctings boiled 1 time 0.5 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds ethanol precipitate with ethanol twice, makes that to contain the alcohol amount be 50% for the first time, make for the second time that to contain the alcohol amount be 80%, filter merging filtrate, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ophiopogonis extract;

B, get the Herba Erigerontis medical material, added 5 times of volumes, 50% alcohol reflux 1 time 0.5 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the ginseng crude drug, add 6 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 3 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 0.5ml/g medical material .min, use 10 times of resinite hydrops and 5 times of resin volume 25% alcohol flushing impurity successively, use 60% alcohol desorption of 4 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

The said extracted thing is merged, add an amount of water for injection dissolving, by volume add 0.1% active carbon, boil, keep little 60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 5.5, boil, 8 ℃ of cold preservations 12 hours, coarse filtration, fine straining, dividing to install in the ampoule bottle, is 110 ℃ in vapor (steam) temperature, and actual pressure is at 120kN/m ³Pressure sterilizing is 60 minutes under the condition, promptly gets the injection with small volume or the concentrated solution for injection that are directly used in drug administration by injection.After testing, to account in the preparation total solid of deduction adjuvant amount and water quantities be 47% to saponin component.

Embodiments of the invention 13: 300 parts of 60 parts of Herba Erigerontiss of 110 parts of Radix Ginseng Rubra Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 8 times of volume decoctings boils 3 times, each 1.5 hours, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.4ml/g medical material .min, water with 6 times of resin volumes washes with the speed of 0.7ml/g medical material .min earlier, 15% ethanol of 4 times of resin volumes of reuse is with the speed eluting impurity of 1.2ml/g medical material .min, use the speed eluting of 70% ethanol of 4 times of resin volumes at last, collect stripping liquid, reclaim ethanol with 0.8ml/g medical material .min, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 4 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.5ml/g medical material .min, use 10 times of resinite hydrops and 6 times of resin volume 15% alcohol flushing impurity successively, use 40% alcohol desorption of 4 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the Radix Ginseng Rubra medical material, add 10 times of volume 70% alcohol reflux 2 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 4 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 0.5ml/g medical material .min, use 7 times of resinite hydrops and 5 times of resin volume 10% alcohol flushing impurity successively, use 60% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng Rubra extract;

The said extracted thing is merged, add an amount of water for injection dissolving, by volume add 0.1%～1.5% active carbon, boil, keep little 10～60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 6.0, boil, 1～8 ℃ of cold preservation 12 hours, coarse filtration, fine straining, divide to install in the enamel tray temperature-45 ℃, pre-freeze time 10h;-40 ℃ of evacuation keep 8h; Be warming up to-30 ℃ again, keep 8h; Be warming up to-20 ℃, keep 8h; Be warming up to-10 ℃, keep 6h; Be warming up to 0 ℃, keep 5h; Be warming up to 10 ℃, keep 2h; Be warming up to 20 ℃, keep 2h, under aseptic condition, divide to install to promptly to get the freeze dry sterile powder end in the cillin bottle.After testing: after testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 3.2% of total solid after deduction adjuvant amount and the water quantities, carbohydrate content content accounts in the preparation 4% of total solid after deduction adjuvant amount and the water quantities, and flavones ingredient content accounts for 42% of the total solid after the deduction adjuvant amount and water quantities in the preparation.

Embodiments of the invention 14: 500 parts of 200 parts of Herba Erigerontiss of 200 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 1.5% active carbon, boil, keep little 60min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, transfer pH value 7.5, boil, 8 ℃ of cold preservations 12 hours, coarse filtration, fine straining, dividing to install in the ampoule bottle, is 110 ℃ in vapor (steam) temperature, and actual pressure is at 120kN/m ³Pressure sterilizing is 60 minutes under the condition, promptly gets the injection with small volume or the concentrated solution for injection that are directly used in drug administration by injection.

The content of carbohydrate content accounts in the preparation 4% of total solid after deduction adjuvant amount and the water quantities.

Embodiments of the invention 15: 200 parts of 50 parts of Herba Erigerontiss of 50 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, add the glucose of ormal weight again, by volume add 0.1% active carbon, boil, keep little 10min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, transfer pH value 5.5, boil, at 1 ℃ of cold preservation 12 hours, coarse filtration, fine straining, add the injection water, packing is under 105 ℃ of conditions, sterilized 20 minutes, and promptly got the glucose intravenous infusion agent.

Embodiments of the invention 16: 1000 parts of 500 parts of Herba Erigerontiss of 500 parts of Radix Ginsengs Radix Ophiopogonis

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, add the sodium chloride of ormal weight again, by volume add 1.5% active carbon, boil, keep little 60min that boils, cold slightly filtration, filtrate add the injection water to ormal weight, transfer pH value 7.5, boil, at 8 ℃ of cold preservations 12 hours, coarse filtration, fine straining, add the injection water, packing is under 125 ℃ of conditions, sterilized 60 minutes, and promptly got the sodium chloride intravenous infusion agent.

Claims

One kind have human body immunity improving power, the treatment cardiovascular and cerebrovascular disease traditional medicine Injectio, it is characterized in that: calculate according to components by weight percent, it is made through extracting refining and adding suitable adjuvant by 200～500 parts of 50～200 parts of 50～200 parts of Radix Ophiopogonis, Radix Ginseng and Herba Erigerontiss, or adding the injection that suitable adjuvant is made through extracting the extract that obtains after refining by corresponding weight portion medical material, the content of carbohydrate content accounts for that the total solid after the deduction adjuvant amount and water quantities is not less than 4% in the preparation in the preparation.
2. according to the described traditional medicine Injectio of claim 1 with human body immunity improving power, treatment cardiovascular and cerebrovascular disease, it is characterized in that: contain saponin component in the effective site Radix Ginseng total saponins of Radix Ginseng and be not less than 50%, contain saponin component in the effective site Radix Ophiopogonis total saponins of Radix Ophiopogonis and be not less than 50%, contain the polysaccharide composition in the another one effective site Radix Ophiopogonis polysaccharide of Radix Ophiopogonis and be not less than 50%, contain flavones ingredient in the effective site Herba Erigerontis total flavones of Herba Erigerontis and be not less than 50%; The total solid that saponin component in the preparation, polysaccharide composition, flavones ingredient sum account in the preparation after deduction adjuvant amount and the water quantities is not less than 25%.
3. the preparation method with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease as claimed in claim 1 is characterized in that:

Radix Ophiopogonis, people participate in Herba Erigerontis three flavor medical materials and add water or ethanol extraction respectively, extracting solution carries out suitably concentrating to such an extent that crude extract also further adopts alcohol deposition method, water precipitating method, one or more methods in acid-base precipitation method, flocculent precipitation, column chromatography, the organic solvent extractionprocess be used in combination refining extract, the refining extract of get it filled material crude extract or medical material adds adjuvant and makes different ejection preparations.
4. the preparation method with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease as claimed in claim 3 is characterized in that:

A, get medical material Radix Ophiopogonis, adding 5～15 times of volume decoctings boils 1～4 time, each 0.5～2.5 hour, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.3-0.8ml/g medical material min, water with 3-10 times of resin volume washes with the speed of 0.5-1.5ml/g medical material min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 50～70%, make for the second time that to contain the alcohol amount be 80～90%, filter, twice precipitation merged the back add 1～4 times of water dissolution, filter, filtrate concentrate Radix Ophiopogonis polysaccharide, the 5-25% ethanol of reuse 1-4 times of resin volume is with the speed eluting impurity of 0.5-1.5ml/g medical material min, at last with the 50-70% ethanol of 2-6 times of resin volume speed eluting with 0.5-1.0ml/g medical material min, collect stripping liquid, get Radix Ophiopogonis total saponins and the merging of above-mentioned Radix Ophiopogonis polysaccharide after reclaiming ethanol, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 5～15 times of volume 50～80% alcohol reflux 1～4 time, each 0.5～2.5 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 1-5 times of medical material volume, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.1-0.8ml/g medical material min, with 1-10 times of resinite hydrops and 1-6 times of resin volume 5-15% alcohol flushing impurity, with the 30-70% alcohol desorption of 1-7 times of resin volume, collect stripping liquid then successively, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the ginseng crude drug, add 5～15 times of volume 50～80% alcohol reflux 1～4 time, each 0.5～2.5 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 1-5 times of medical material volume, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 0.3-1.5ml/g medical material min, with 1-10 times of resinite hydrops and 1-6 times of resin volume 5-15% alcohol flushing impurity, with the 30-70% alcohol desorption of 1-7 times of resin volume, collect stripping liquid then successively, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add adjuvant and make different ejection preparations.
5. according to the described preparation method of claim 4, it is characterized in that with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease:

A, get medical material Radix Ophiopogonis, adding 8 times of volume decoctings boils 3 times, each 1 hour, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.5ml/g medical material min, water with 6 times of resin volumes washes with the speed of 1ml/g medical material min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 60%, make for the second time that to contain the alcohol amount be 85%, filter, will twice precipitation merge the back and add 2 times of water dissolutioies, filter, measuring relative density when filtrate decompression is concentrated into 60 ℃ is 1.05～1.15, gets Radix Ophiopogonis polysaccharide, and 20% ethanol of 3 times of resin volumes of reuse is with the speed eluting impurity of 1ml/g medical material min, use the speed eluting of 60% ethanol of 4 times of resin volumes at last with 0.8ml/g medical material min, collect stripping liquid, get Radix Ophiopogonis total saponins and the merging of above-mentioned Radix Ophiopogonis polysaccharide behind the recovery ethanol, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 3 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.2ml/g medical material min, use 5 times of resinite hydrops and 4 times of resin volume 10% alcohol flushing impurity successively, use 40% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry the thin total flavones of oil lamp;

C, get the ginseng crude drug, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 4 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 1ml/g medical material min, use 7 times of resinite hydrops and 5 times of resin volume 10% alcohol flushing impurity successively, use 60% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add adjuvant and make different ejection preparations.
6. according to the described preparation method with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease of claim 5, it is characterized in that: aseptic block is preparation like this:

A, get medical material Radix Ophiopogonis, adding 8 times of volume decoctings boils 3 times, each 1 hour, merge extractive liquid,, filter, filtrate is crossed ZTC-1 type macroporous adsorptive resins with the speed of 0.5ml/g medical material min, water with 6 times of resin volumes washes with the speed of 1ml/g medical material min earlier, sample effluent and water lotion in the collection, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds the ethanol precipitate with ethanol twice, make for the first time that to contain the alcohol amount be 60%, make for the second time that to contain the alcohol amount be 85%, filter, will twice precipitation merge the back and add 2 times of water dissolutioies, filter, measuring relative density when filtrate decompression is concentrated into 60 ℃ is 1.05～1.15, gets Radix Ophiopogonis polysaccharide, and 20% ethanol of 3 times of resin volumes of reuse is with the speed eluting impurity of 1ml/g medical material min, use the speed eluting of 60% ethanol of 4 times of resin volumes at last with 0.8ml/g medical material min, collect stripping liquid, get Radix Ophiopogonis total saponins and the merging of above-mentioned Radix Ophiopogonis polysaccharide behind the recovery ethanol, the dry Radix Ophiopogonis extract that gets;

B, get the Herba Erigerontis medical material, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water heating for dissolving that adds 3 times of medical material volumes, filter, filtrate is crossed AB-8 type macroporous adsorbent resin with the speed of 0.2ml/g medical material min, use 5 times of resinite hydrops and 4 times of resin volume 10% alcohol flushing impurity successively, use 40% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Herba Erigerontis total flavones;

C, get the ginseng crude drug, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, the water dissolution that adds 4 times of medical material volumes, filter, filtrate is crossed ZTC-1 type macroporous adsorbent resin with the speed of 1ml/g medical material min, use 7 times of resinite hydrops and 5 times of resin volume 10% alcohol flushing impurity successively, use 60% alcohol desorption of 5 times of resin volumes then, collect stripping liquid, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Radix Ginseng total saponins;

Above-mentioned Radix Ophiopogonis extract, Herba Erigerontis total flavones and Radix Ginseng total saponins are merged, add an amount of water for injection dissolving, by volume add 1.0% active carbon, boil, keep little 30min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, and adjust pH 5.5～7.5 boils, at 4 ℃ of cold preservations 12 hours, coarse filtration, fine straining; Suitable adjuvant is added the injection water is mixed with solution,, filter with above-mentioned filtrate mixing, packing, temperature-45 ℃, pre-freeze time 10h, the beginning evacuation, and in 12～72 hours differential gradient increased temperature to 10 ℃ progressively, keep 2h, be warming up to 20 ℃, keep 2h, promptly.