CN1911383A

CN1911383A - Injection contg. traditional Chinese medicine, and its prepn. method

Info

Publication number: CN1911383A
Application number: CN 200510090419
Authority: CN
Inventors: 于文风
Original assignee: Union Xichuang Pharmaceutical Science & Tech Co Ltd Beijing
Current assignee: Union Xichuang Pharmaceutical Science & Tech Co Ltd Beijing
Priority date: 2005-08-12
Filing date: 2005-08-12
Publication date: 2007-02-14

Abstract

A Chinese medicine in the form of injection for improving immunity and treating cardiovascular and cerebrovascular diseases, such as coronary heart disease, angina pectoris, arrhythmia, cerebral infarction and senile dementia, is prepared from ophiopogon root, ginseng or red ginseng or pilose asiabell root, schisandra fruit and shortscape fleabane herb. Its preparing process is also disclosed, which features the purifying by organic solvent.

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 suit the medicine to the illness--and-cardiovascular and cerebrovascular disease is a big persistent ailment that threatens world's healthy population as coronary heart disease, myocardial infarction, rhomboembolia type cerebrovascular, and the trend that progressively rises is arranged in recent years.The height of cardiovascular and cerebrovascular disease mortality rate is to weigh a country, resident's quality of life, the important indicator of sanitary health career, along with the arriving of fairly comfortable life, and the change of meals spectrum, resident's longevity, healthy existence desire improve constantly.In order to prevent, control the generation of cardiovascular and cerebrovascular disease, exploitation cardiovascular and cerebrovascular disease class medicine has become a main trend.Therefore, it is low to seek a kind of cost, determined curative effect, and the natural Chinese medicines preparation that has no side effect is very urgent, contrast after deliberation, we develop a kind of ejection preparation for the treatment of cardiovascular and cerebrovascular disease, are made up of Radix Ophiopogonis, Radix Ginseng, Herba Erigerontis and Fructus Schisandrae Chinensis.Many inventors have also done number of research projects, as: number of patent application is " 02153750.X ", name is called the application of " a kind of Herba Erigerontis combination drug ", though the product of this part application has good clinical application effect, but the harm that cardiovascular and cerebrovascular disease acute attack at present brings to human health is bigger, oral formulations can't discharge medicine rapidly, lie in a comatose condition owing to the patient simultaneously, dysphagia, medicine disintegrate in gastrointestinal tract in addition, absorption are individual processes slowly, therefore can't reach the curative effect that needs.In view of such circumstances, seek a kind of therapeutic effect ideal, the thing that medicine preparation stable and controllable for quality has just become people to be badly in need of solving.

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 is directed to prior art, at different medical materials, adopt the mode of separately extracting, both can effectively extract active component, simultaneously can be under the situation that guarantees active component, remove impurity targetedly, sample is made with extra care, add that the treatment of cardiovascular and cerebrovascular disease acute attack stage is extremely important, preparation of the present invention is mainly injection, make medicine performance curative effect fast, the availability height is fit to the treatment of cardiovascular and cerebrovascular disease.

Technical solution of the present invention is achieved in that a kind of traditional medicine Injectio with human body immunity improving power, treatment cardiovascular and cerebrovascular disease: calculate according to parts by weight, it is made through extracting refining and adding suitable adjuvant by 50～1000 parts of 1～300 part of 10～500 parts of Radix Ophiopogonis, 1～300 part of Radix Ginseng, Fructus Schisandrae Chinensis and Herba Erigerontiss, or add suitable adjuvant and be made through extracting the extract that obtains after refining by corresponding weight portion medical material, contain the various saccharides composition in the preparation, and do not extract the volatile oil composition of Fructus Schisandrae Chinensis separately.Described 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 200～500 parts of 10～100 parts of 50～200 parts of Radix Ophiopogonis, 10～100 parts of Radix Ginsengs, Fructus Schisandrae Chinensis and Herba Erigerontiss, or add suitable adjuvant and be made through extracting the extract that obtains after refining by corresponding weight portion medical material, contain various saccharides compositions such as Radix Ophiopogonis polysaccharide and monosaccharide in the preparation, and do not extract the volatile oil composition of Fructus Schisandrae Chinensis separately.Say exactly, it is to be made through extracting refining and adding suitable adjuvant by 300 parts of 60 parts of 110 parts of Radix Ophiopogonis, 60 parts of Radix Ginsengs, Fructus Schisandrae Chinensis and Herba Erigerontiss, or add suitable adjuvant and be made through extracting the extract that obtains after refining by corresponding weight portion medical material, contain various saccharides compositions such as Radix Ophiopogonis polysaccharide and monosaccharide in the preparation, calculate according to weight ratio, the total solid that the content of carbohydrate content accounts in the preparation after deduction adjuvant amount and the water quantities is not less than 4%, and does not extract the volatile oil composition of Fructus Schisandrae Chinensis separately.

The Radix Ginseng that the present invention relates to can also be the Radix Ginseng Rubra or the Radix Codonopsis of equivalent.

Preparation of the present invention is an injection, comprising: be directly used in drug administration by injection injection, need to be used for after the dilution concentrated solution for injection of intravenous drip, directly for the glucose intravenous infusion of intravenous drip and sodium chloride intravenous infusion and the injectable sterile powder and the aseptic block that make with freeze-drying or spray drying method.

Contain saponin component, polysaccharide composition and flavones ingredient in the preparation of the present invention, calculate according to weight ratio, 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%, the total solid that the content of polysaccharide composition accounts in the preparation after deduction adjuvant amount and the water quantities is not less than 3%, and all can survey the 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.

The preparation method of traditional medicine Injectio of the present invention is: Radix Ophiopogonis, Radix Ginseng, Fructus Schisandrae Chinensis and Herba Erigerontis four Chinese medicine material add water or ethanol extraction respectively, extracting solution carry out suitably concentrating crude extract or further adopt one or more methods in alcohol deposition method, acid-base precipitation method, column chromatography, the solvent extraction to mix to use refining extract, add different auxiliary material and make various ejection preparations.

Specifically: the preparation method of traditional medicine Injectio of the present invention is:

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,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add 1～4 times of amount n-butyl alcohol, shaking out 1～8 time, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, and the water liquid after the extraction adds 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, will twice precipitation merge the back and add 1～4 times of water dissolution, filter, the concentrated solution of filtrate and front merges, and measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get schisandra chinensis medicinal material, add 5～15 times of volume water boiling and extraction 1～4 time, each 0.5～2.5 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 1～4 times of amount ethyl acetate, shaking out 1～8 time, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, 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, measuring relative density when merge extractive liquid,, decompression and solvent recovery to 60 ℃ is 1.05～1.15, adds 1～4 times and measures ethyl acetate, shaking out 1～8 time, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, 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 when being concentrated into 60 ℃ is 1.05～1.15, adds 1～4 times of amount n-butyl alcohol, shaking out 1～8 time, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Radix Ginseng extract;

Above-mentioned Radix Ophiopogonis extract, Fructus Schisandrae Chinensis extrat, Herba Erigerontis extract and Radix Ginseng extract are merged, add adjuvant and make different ejection preparations.

Injection of the present invention prepares like this:

A, get medical material Radix Ophiopogonis, adding 10 times of volume decoctings boils 3 times, each 1.5 hours, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 2 times of amount n-butyl alcohol, shaking out 5 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, and the water liquid after the extraction 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, the concentrated solution of filtrate and front merges, and measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get schisandra chinensis medicinal material, add 10 times of volume water boiling and extraction 3 times, each 1.5 hours, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 1 times of amount ethyl acetate, shaking out 4 times, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, get the Herba Erigerontis medical material, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 2 times of amount ethyl acetate, shaking out 5 times, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, get the ginseng crude drug, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 2 times of amount n-butyl alcohol, shaking out 5 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Radix Ginseng extract;

Above-mentioned Radix Ophiopogonis extract, Fructus Schisandrae Chinensis extrat, Herba Erigerontis extract and Radix Ginseng extract 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, spend the night coarse filtration, fine straining 1～8 ℃ of cold preservation.Mannitol is added the injection water be mixed with 50～150mg/ml solution,, filter packing with above-mentioned filtrate mixing, 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, promptly get freeze-dried powder.

The adjuvant that is adopted in the preparation process 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.

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

A, Radix Ophiopogonis medical material, adding 10 times of volume decoctings boils 3 times, each 1.5 hours, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 2 times of amount n-butyl alcohol, shaking out 5 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, and the water liquid after the extraction 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, the concentrated solution of filtrate and front merges, and measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

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 5.5～7.5, boil, spend the night 1～8 ℃ of cold preservation, 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.

The glucose intravenous infusion agent is preparation like this in the injection of the present invention:

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%～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, spend the night coarse filtration, fine straining 1～8 ℃ of cold preservation, add the injection water, packing is under 105～125 ℃ of conditions, sterilized 20～60 minutes, and promptly got the glucose intravenous infusion agent.

The sodium chloride intravenous infusion agent is preparation like this in the injection of the present invention:

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 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, spend the night coarse filtration, fine straining 1～8 ℃ of cold preservation, add the injection water, packing is under 105～125 ℃ of conditions, sterilized 20～60 minutes, and promptly got the sodium chloride intravenous infusion agent.

Injection of the present invention prepares like this:

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 5.5～7.5, boil, spend the night 1～8 ℃ of cold preservation, 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.

The spray drying sterilized powder is preparation like this in the injection of the present invention:

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 5.5～7.5, boil, spend the night 1～8 ℃ of cold preservation, 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 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 pharmacological research conclusion

Of the present invention group of SHENGMAI ZHUSHEYE group of pilot project breviscapus pulse-engendering Capsules group

Heart effect is remarkable due to the dog coronary artery ligation method, and the general effect of effect reinforced effects is general

The muscle infarction model test

It is remarkable to improve blood stasis model rat serum liquid stream effect, and effect reinforced effects positive effect is general

Denatured test

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

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

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

The not obvious DeGrain of effect remarkable result during the survival of white mice normal pressure anoxia enduring

Between test

From above-mentioned test as can be seen, therefore the injection therapeutic effect proves that said preparation is effective significantly better than oral direct.

Experimental example 2: injection with small volume or concentrated solution for injection molding research

(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 8.68 54.01 is reddish brown

1 8.37 53.69 is red

1.5 8.42 48.76 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 8.35 52.62 is reddish brown

30 8.26 52.18 is red

60 8.37 50.82 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.

(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 5.2 5.8 6.3 6.6 7.2 7.7 8.2

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

The result shows, medicinal liquid boils the back pH value and occurs precipitating at the sample 5.5 below, 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, be 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 5.26 5.2 5.21

2 6.0 5.26 5.7 5.23

3 6.5 5.26 6.2 5.19

4 7.0 5.26 6.6 5.20

5 7.5 5.26 7.2 5.27

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 3: the investigation of freeze-dry process

(1) 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 solubility finished product outward appearance

(V∶V)

2: 1 good parts of glucose subside

Galactose general molding in 2: 1

Mannitol good molding in 2: 1

Glycine good molding in 2: 1, frangible

Dextran general molding in 2: 1

Mannitol, propylene glycol good molding in 2: 1

Glycine, Polyethylene Glycol good molding in 2: 1, frangible

Dextran, sorbitol, tween good molding in 2: 1

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.

(2) caffolding agent consumption screening

The mannitol solution (50mg/ml, 100mg/ml and 150mg/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 color and luster profile solubility clarity

Numbering

(mg/ml) (v∶v)

1 50 2: 1 yellowish-brown part has been subsided up to specification

2 100 2: 1 is yellow intact good up to specification

3 150 2: 1 is yellowish intact good up to specification

As seen from table, when the ratio of caffolding agent consumption and medicinal liquid is 2: 1, the sample character is that the sample of 100mg/ml and 150mg/ml is relatively good with the mannitol concentration, the sample of 50mg/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 2: 1.

(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)

Temperature (℃) condition I condition II condition III cold-trap

-45 (pre-freezes) 8-8

-40 (pre-freeze)-8-

-40 (evacuation) 8-10

-35 (evacuation)-8-

-30 (evacuation) 8-10 keeps

-25 (evacuation)-8--70 ℃

-20 (evacuation) 8-10

-15 (evacuation)-8-

-10 (evacuation) 5-5

0 (evacuation) 555

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 5h; 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 4: 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 4.26

150 70 18 2.78

160 80 20 3.02

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: 1000 parts of 300 parts of Herba Erigerontiss of 300 parts of Fructus Schisandrae Chinensis of 500 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,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 4 times of amount n-butyl alcohol, shaking out 8 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, and the water liquid after the extraction 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, the concentrated solution of filtrate and front merges, and measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get schisandra chinensis medicinal material, add 15 times of volume water boiling and extraction 4 times, each 2.5 hours, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 4 times of amount ethyl acetate, shaking out 8 times, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, get the Herba Erigerontis medical material, add 15 times of volume 80% alcohol reflux 4 times, each 2.5 hours, measuring relative density when merge extractive liquid,, decompression and solvent recovery to 60 ℃ is 1.05～1.15, adds 4 times and measures ethyl acetate, shaking out 8 times, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, 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 when being concentrated into 60 ℃ is 1.05～1.15, adds 4 times of amount n-butyl alcohol, shaking out 8 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Radix Ginseng extract;

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 5.5～7.5, boils, and spends the night coarse filtration, fine straining 4 ℃ of cold preservations.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 5h; 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 40% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 20% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 30% 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 2: 50 parts of 1 part of Herba Erigerontiss of 1 part of Fructus Schisandrae Chinensis 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, add 1 times of amount n-butyl alcohol, shaking out 1 time merges n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, water liquid after the extraction adds ethanol precipitate with ethanol twice, makes that to contain the alcohol amount be 50% for the first time, makes that to contain the alcohol amount be 80% for the second time, filter, twice precipitation merged the back add 1 times of water dissolution, filter, the concentrated solution of filtrate and front merges, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get schisandra chinensis medicinal material, added 5 times of volume water boiling and extraction 1 time 0.5 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add 1 times of amount ethyl acetate, shaking out 1 time, combined ethyl acetate liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, 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 and solvent recovery to 60 ℃ is 1.05～1.15, add 1 times of amount ethyl acetate, shaking out 1 time, combined ethyl acetate liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, get the ginseng crude drug, 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, add 1 times of amount n-butyl alcohol, shaking out 1 time merges n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Radix Ginseng extract;

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 5.5～7.5, boil, spend the night 8 ℃ of cold preservations, 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 20% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 2% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 3% 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 3: 300 parts of 60 parts of Herba Erigerontiss of 60 parts of Fructus Schisandrae Chinensis of 110 parts of Radix Ginsengs Radix Ophiopogonis

A, Radix Ophiopogonis medical material, 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, add 1 times of amount n-butyl alcohol, shaking out 1 time merges n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, water liquid after the extraction adds ethanol precipitate with ethanol twice, makes that to contain the alcohol amount be 50% for the first time, makes that to contain the alcohol amount be 80% for the second time, filter, twice precipitation merged the back add 4 times of water dissolutioies, filter, the concentrated solution of filtrate and front merges, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

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 5.5～7.5, boil, spend the night coarse filtration, fine straining 1 ℃ of cold preservation, 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 80% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 2% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 3% of total solid after deduction adjuvant amount and the water quantities.

Embodiments of the invention 4: 60 parts of Herba Erigerontiss 300 of 60 parts of Fructus Schisandrae Chinensis of 110 parts of Radix Ginsengs Radix Ophiopogonis

A, get medical material Radix Ophiopogonis, adding 10 times of volume decoctings boils 2 times, each 1 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 2 times of amount n-butyl alcohol, shaking out 4 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, and the water liquid after the extraction 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 90%, filter, will twice precipitation merge the back and add 2 times of water dissolutioies, filter, the concentrated solution of filtrate and front merges, and measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get schisandra chinensis medicinal material, added 10 times of volume water boiling and extraction 1 time 0.5 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, add 1 times of amount ethyl acetate, shaking out 1 time, combined ethyl acetate liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, get the Herba Erigerontis medical material, add 12 times of volume 70% alcohol reflux 3 times, each 1 hour, measuring relative density when merge extractive liquid,, decompression and solvent recovery to 60 ℃ is 1.05～1.15, adds 2 times and measures ethyl acetate, shaking out 5 times, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, get the ginseng crude drug, add 8 times of volume 600% alcohol reflux 3 times, each 1.5 hours, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 2 times of amount n-butyl alcohol, shaking out 4 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Radix Ginseng extract;

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 5.5～7.5, boil, spend the night coarse filtration, fine straining 4 ℃ of cold preservations, add the injection water, packing is under 115 ℃ of conditions, sterilized 30 minutes, and promptly got the sodium chloride intravenous infusion agent.After testing: Radix Ophiopogonis polysaccharide content accounts in the preparation 30% of total solid after deduction adjuvant amount and the water quantities; The content of saponin component accounts in the preparation 10% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 20% of total solid after deduction adjuvant amount and the water quantities.

Embodiments of the invention 5: 30 parts of 6 parts of Herba Erigerontiss of 6 parts of Fructus Schisandrae Chinensis of 11 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, add 2 times of amount n-butyl alcohol, shaking out 4 times merges n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, water liquid after the extraction adds ethanol precipitate with ethanol twice, makes that to contain the alcohol amount be 60% for the first time, makes that to contain the alcohol amount be 90% for the second time, filter, twice precipitation merged the back add 2 times of water dissolutioies, filter, the concentrated solution of filtrate and front merges, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get schisandra chinensis medicinal material, add 10 times of volume water boiling and extraction 2 times, each 1..5 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of amount ethyl acetate, shaking out 2 times, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, get the Herba Erigerontis medical material, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, measuring relative density when merge extractive liquid,, decompression and solvent recovery to 60 ℃ is 1.05～1.15, adds 3 times and measures ethyl acetate, shaking out 4 times, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, get the ginseng crude drug, adding 10 times of volume decoctings boils 3 times, each 1.5 hours, measuring relative density when merge extractive liquid, is concentrated into 60 ℃ is 1.05～1.15, add 2 times of amount n-butyl alcohol, shaking out 4 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, and the water liquid after the extraction 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, will twice precipitation merges the back and adds 1 times of water dissolution, filter, the concentrated solution of filtrate and front merges, and measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ginseng extract that gets.The dry Radix Ginseng extract that gets;

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 5.5～7.5, boil, spend the night 1～8 ℃ of cold preservation, 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 5h; 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: polyoses content accounts in the preparation 50% of total solid after deduction adjuvant amount and the water quantities, still contains the ginseng polysaccharide except that containing Radix Ophiopogonis polysaccharide; The content of saponin component accounts in the preparation 5% of total solid after deduction adjuvant amount and the water quantities; The content of flavones ingredient accounts in the preparation 15% of total solid after deduction adjuvant amount and the water quantities.

Embodiments of the invention 6: 30 parts of 6 parts of Herba Erigerontiss of 6 parts of Fructus Schisandrae Chinensis of 11 parts of Radix Codonopsis Radix Ophiopogonis

B, get schisandra chinensis medicinal material, added 5 times of volume water boiling and extraction 1 time 0.5 hour, measuring relative density when extracting solution is concentrated into 60 ℃ is 1.05～1.15, add 1 times of amount ethyl acetate, shaking out 1 time, measuring relative density when combined ethyl acetate liquid, decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, get the Herba Erigerontis medical material, added 5 times of volumes, 50% alcohol reflux 1 time 0.5 hour, extracting solution, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, add 1 times of amount ethyl acetate, shaking out 1 time, combined ethyl acetate liquid, measuring relative density during decompression and solvent recovery to 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, get codonopsis pilosula, add 8 times of volume 600% alcohol reflux 3 times, each 1.5 hours, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 2 times of amount n-butyl alcohol, shaking out 4 times, merge n-butyl alcohol liquid, measuring relative density during decompression and solvent recovery 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, spend the night 6 ℃ of cold preservations, 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 7: 50 parts of 1 part of Herba Erigerontiss of 1 part of Fructus Schisandrae Chinensis 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 schisandra chinensis medicinal material, added 5 times of volume water boiling and extraction 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 Fructus Schisandrae Chinensis extrat;

C, 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 extract;

D, get the ginseng crude drug, 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 Radix Ginseng extract;

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 ~ 7.5, boil, spend the night 8 ℃ of cold preservations, 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 3% of total solid after deduction adjuvant amount and the water quantities.

Embodiments of the invention 8: 30 parts of 6 parts of Herba Erigerontiss of 6 parts of Fructus Schisandrae Chinensis of 11 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,, 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, and 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, reclaim ethanol, measuring relative density when being evaporated to 60 ℃ is 1.05～1.15, the dry Radix Ophiopogonis extract that gets;

B, get schisandra chinensis medicinal material, add 10 times of volume water boiling and extraction 3 times, each 1.5 hours, merge extractive liquid,, 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 merging filtrate, measuring relative density during decompression recycling ethanol to 60 ℃ is 1.05～1.15, dry Fructus Schisandrae Chinensis extrat;

C, get the Herba Erigerontis medical material, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, dry Herba Erigerontis extract;

D, 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 5.5 ~ 7.5, boil, spend the night 1～8 ℃ of cold preservation, 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 5h; 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: carbohydrate content content accounts in the preparation 4% of total solid after deduction adjuvant amount and the water quantities, and polyoses content accounts for 3% of the total solid after the deduction adjuvant amount and water quantities in the preparation.

Claims

1, a kind of traditional medicine Injectio with human body immunity improving power, treatment cardiovascular and cerebrovascular disease, it is characterized in that: calculate according to components by weight percent, it is made through extracting refining and adding suitable adjuvant by 50～1000 parts of 1～300 part of 10～500 parts of Radix Ophiopogonis, 1～300 part of Radix Ginseng, Fructus Schisandrae Chinensis and Herba Erigerontiss, or add suitable adjuvant and be made through extracting the extract that obtains after refining by corresponding weight portion medical material, contain the various saccharides composition in the preparation, and do not extract the volatile oil composition of Fructus Schisandrae Chinensis separately.

2, has human body immunity improving power according to claim 1 is described, the traditional medicine Injectio of treatment cardiovascular and cerebrovascular disease, it is characterized in that: calculate according to components by weight percent, it is by 50～200 parts of Radix Ophiopogonis, 10～100 parts of Radix Ginsengs, 200～500 parts of 10～100 parts of Fructus Schisandrae Chinensis and Herba Erigerontiss are through extracting refining and adding the injection that suitable adjuvant is made, or add suitable adjuvant and be made through extracting the extract that obtains after refining by corresponding weight portion medical material, contain various saccharides compositions such as Radix Ophiopogonis polysaccharide and monosaccharide in the preparation, and do not extract the volatile oil composition of Fructus Schisandrae Chinensis separately.

3, describedly has human body immunity improving power according to claim 1 or 2, the traditional medicine Injectio of treatment cardiovascular and cerebrovascular disease, it is characterized in that: calculate according to components by weight percent, it is by 110 parts of Radix Ophiopogonis, 60 parts of Radix Ginsengs, 300 parts of 60 parts of Fructus Schisandrae Chinensis and Herba Erigerontiss are through extracting refining and adding the injection that suitable adjuvant is made, or the extract that is obtained after extracting by corresponding weight portion medical material is through refining and add the injection that suitable adjuvant is made, contain various saccharides compositions such as Radix Ophiopogonis polysaccharide and monosaccharide in the preparation, calculate according to weight ratio, the total solid that the content of carbohydrate content accounts in the preparation after deduction adjuvant amount and the water quantities is not less than 4%, and does not extract the volatile oil composition of Fructus Schisandrae Chinensis separately.

4, according to any described traditional medicine Injectio with human body immunity improving power, treatment cardiovascular and cerebrovascular disease of claim 1-3, it is characterized in that: injection comprises: be directly used in drug administration by injection injection, need to be used for after the dilution concentrated solution for injection of intravenous drip, directly for the glucose intravenous infusion of intravenous drip and sodium chloride intravenous infusion and the injectable sterile powder and the aseptic block that make with freeze-drying or spray drying method.

5, according to the described traditional medicine Injectio of claim 4 with human body immunity improving power, treatment cardiovascular and cerebrovascular disease, it is characterized in that: contain saponin component, polysaccharide composition and flavones ingredient in the preparation, calculate according to weight ratio, 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 the content of polysaccharide composition accounts for that the total solid after the deduction adjuvant amount and water quantities is not less than 3% in the preparation.

6, according to the described traditional medicine Injectio of claim 5 with human body immunity improving power, treatment cardiovascular and cerebrovascular disease, it is characterized in that: calculate according to weight ratio, all can survey the 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.

7, the preparation method with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease as claimed in claim 4, it is characterized in that: Radix Ophiopogonis, Radix Ginseng, Fructus Schisandrae Chinensis and Herba Erigerontis four Chinese medicine material add water or ethanol extraction respectively, extracting solution carry out suitably concentrating crude extract or further adopt one or more methods in alcohol deposition method, acid-base precipitation method, column chromatography, the solvent extraction to mix to use refining extract, extract or refining extract adds adjuvant and makes different ejection preparations medical material is thick.

8, the preparation method with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease as claimed in claim 7 is characterized in that:

9, according to the described preparation method of claim 8, it is characterized in that with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease:

10, according to the described preparation method with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease of claim 9, it is characterized in that: lyophilized injectable powder is preparation like this:

Above-mentioned Radix Ophiopogonis extract, Fructus Schisandrae Chinensis extrat, Herba Erigerontis extract and Radix Ginseng extract 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, spend the night coarse filtration, fine straining 4 ℃ of cold preservations.Suitable adjuvant is added the injection water be mixed with solution,, filter packing with above-mentioned filtrate mixing, 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 get lyophilized injectable powder.

11, according to any described preparation method with traditional medicine Injectio of human body immunity improving power, treatment cardiovascular and cerebrovascular disease among the claim 7-10, it is characterized in that: the adjuvant that is adopted in the preparation comprises one or more in mannitol, galactose, glycine, glucose, sodium chloride, dextran, glycerol, ethanol, propylene glycol, Polyethylene Glycol, sorbitol, tween, the poloxamer.

12, according to claim 1-3 and any described traditional medicine Injectio with human body immunity improving power, treatment cardiovascular and cerebrovascular disease of 7-10, it is characterized in that: Radix Ginseng can also be the Radix Ginseng Rubra or the Radix Codonopsis of equivalent.