CN1284526C - Method for preparing powdered injection of 'Shuanghuanglian' formulation - Google Patents
Method for preparing powdered injection of 'Shuanghuanglian' formulation Download PDFInfo
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Abstract
The present invention relates to a method for preparing powdered 'Shuanghuanglian' formulation for injection, which is a method for preparing a kind of freeze-dried injection with traditional Chinese medicines. The existing freeze-drying method has the defects of low medicine yield and difficult control over medicine quality, and the prepared medicines have bad clinical curative effects and much adverse reaction. In the preparation method of the present invention, materials are prepared by weight according to the following proportion: 1 portion of honeysuckle, 2 portions of fructus forsythiae and 1 portion of baikal skullcap root, the three kinds of crude medicines are then prepared after being respectively extracted and mixed, and powdered 'Shuanghuanglian' formulation for injection is obtained. Since the powdered 'Shuanghuanglian' formulation for injection, which is prepared with the freeze-drying method, in the present invention is dried at low temperature, the effective constituents of the medicine can not be destroyed easily, the clinical curative effect is good, and medicine particles are maintained in the original state and can be easily dissolved. In addition, the powdered 'Shuanghuanglian' formulation for injection, which is prepared with the method of the present invention, has the advantages of good clinical curative effect and low adverse reaction, and is beneficial for popularization.
Description
Technical field:
The present invention relates to a kind of preparation method of Chinese medicine freeze dried injection.
Background technology:
ZHUSHEYONG SHUANGHUANGLIAN has aqueous injection, injectable powder, and aqueous injection exists cracky, long preservation in poor stability, the transportation to be prone to the drawback of turbidity sediment; The preparation of injectable powder has spray drying method, freeze drying process, and the spray drying method is at high temperature to spray driedly, so the drug moiety active ingredient is easily destroyed, and has increased the chance to drug contamination, and drug microparticles easily produces and gathers, and causes to be difficult for dissolving, thereby influences drug effect; There is the defective that drug quality is wayward, output is not high in existing freeze drying process, and the clinical drug curative effect of preparation is bad, untoward reaction is many.
Summary of the invention:
The preparation method of the dual coptis powder injection that the object of the present invention is to provide that a kind of quality is controlled easily, output height and clinical efficacy is good, its preparation method is as follows: the ratio of 1 part of extracting honeysuckle, 2 parts of Fructus Forsythiaes, 1 part of Radix Scutellariae is prepared material by weight, respectively according to following method preparation:
A. the preparation of Fructus Forsythiae: the A-a. Fructus Forsythiae was soaked 20～40 minutes, decocts 2～3 times, and each 1 hour, merging filtrate; A-b. filter, the clear paste of proportion 1.20-1.25 when heating is concentrated into 70-80 ℃ adds the gelatin that accounts for input raw medicinal herbs weight 0.5% again; When A-c. being cooled to 35-40 ℃, slowly add the ethanol that mass concentration is 90%-95%, stir fully simultaneously, make to contain alcohol amount and reach more than 80%, stop to stir; A-d. refrigeration cool-down is incubated cold preservation 24～48 hours to 0-5 ℃; A-e. the leaching supernatant returns alcohol and concentrates, and the distilled water that adds meltage stirs; A-f. be incubated 0-5 ℃ and placed 24～48 hours, leaching supernatant, the clear paste of proportion 1.1-1.15 when heating is concentrated into 70-80 ℃; A-g. be warming up to 35-40 ℃, stir, slowly add the ethanol of mass concentration 94% or more, make to contain the alcohol amount and reach more than 90%, stop stirring; A-h. be chilled to 0-5 ℃, insulation cold preservation 24～48 hours; A-i. the leaching supernatant returns alcohol and concentrates, and the distilled water that adds meltage stirs; A-j. keep temperature 0-5 ℃ to place after 24～48 hours, the leaching supernatant, the clear paste of proportion 1.1-1.15 was Fructus Forsythiae extractum when heating was concentrated into 70-80 ℃, and is standby;
B. the preparation of Flos Lonicerae: the distinctive points of preparation method of Flos Lonicerae and A step is that in the A-b step, the gelatin amount of adding accounts for and drops into 0.6% of raw medicinal herbs weight; Added following process before A-f step, A-j step respectively: " the NaOH solution that slowly adds deployed mass concentration 10% is transferred PH=5, is heated to boiling, is incubated 27～33 minutes; " gains are Flos Lonicerae extractum;
C. the preparation of Radix Scutellariae: C-a. gets Radix Scutellariae section and decocts with water 2-3 time, and each 1 hour, gradation filtration, merging filtrate; C-b. filtrate was regulated pH value to 1.0～2.0 with the hydrochloric acid of 2mol/L, 80 ℃ of insulations 30 minutes; C-c. be chilled to 0-7 ℃ and left standstill 12-48 hour, filter, precipitate adds 8 times of water gagings, stirs; C-d. the sodium hydroxide solution that slowly adds mass concentration 40% is regulated pH value to 7.0; C-e. slowly adding the ethanol of mass concentration more than 95% makes and contains alcohol amount and reach 50%, stirring and dissolving; C-f. filter, filtrate is regulated pH value to 2.0 with the hydrochloric acid of 2mol/L, and 60 ℃ are incubated 30 minutes; C-g. be chilled to 0-5 ℃ and leave standstill more than 12 hours, filter; C-h. to be washed till pH value with the ethanol of mass concentration more than 90% be 4.0 to precipitate, adds the water that accounts for 10 times of amounts of precipitate, stirs; C-i. be that 40% sodium hydroxide solution is regulated pH value to 7.0 with mass concentration; C-j. add active carbon, make active carbon content account for 0.5% of gross weight, fully stir, 50 ℃ are incubated 30 minutes; C-k. slowly adding the ethanol of mass concentration more than 95% makes and contains alcohol amount and reach 50%; C-l. filter immediately after stirring, filtrate is regulated pH value to 2.0 with the hydrochloric acid of 2mol/L, and 60 ℃ are incubated 30 minutes; C-m. be chilled to 0-5 ℃, left standstill 12 hours, filter; C-n. after precipitate was measured 95% washing with alcohol with 1 times, in dry below 60 ℃, it was standby to get baicalin;
Water fully kneads into the suspendible shape with baicalin, NaOH aqueous solution with mass concentration 6% is transferred pH value to 6.0～7.0, with Flos Lonicerae extractum, Fructus Forsythiae extractum and baicalin mix homogeneously, add concentration and transfer PH6.5～7.2 then, add water for the 6%NaOH aqueous solution, boiling sterilization 30 minutes, fill, the freeze dryer of packing into is set to-45 ℃ with the flaggy temperature, 2～3 hours, and then setting flaggy temperature is-10 ℃ of distillations; The distillation time is 25～30 hours, and resetting the flaggy temperature is 50 ℃, 3 hours rear pressing covers, and packing is promptly.
The SHUANGHUANGLIAN FENZHENJI that the present invention adopts freeze drying process to make, because of dry at low temperatures, so that the active ingredient of medicine is difficult for is destroyed, clinical efficacy is good, and drug microparticles maintains the original state, and dissolves easily; Preparation method advanced person of the present invention, every flavor medicine and intermediate all have content's index control, and assay all adopts high performance liquid chromatography to detect, and has increased finger printing; The present invention is that three kinds of crude drug extract respectively, and system easy to control the quality like this, output height are profitable; Have repugnancy in the preparation process of Flos Lonicerae of the present invention and two kinds of medicines of Fructus Forsythiae, promptly Flos Lonicerae is regulated pH value with water precipitating in preparation process, can more effectively remove impurity like this; The present invention emphasizes that sodium hydroxide, ethanol need " slowly " in adition process in preparation process because can avoid local response acute excessively like this, and when mixing easier mix homogeneously; In the preparation process of Radix Scutellariae of the present invention, emphasizing more than once " being chilled to 0-5 ℃ " is because can more effectively make baicalin separate out in this temperature range; The a large amount of experiment confirms of our warp, the dual coptis powder injection that the inventive method is produced, clinical efficacy is good, and untoward reaction is few, is beneficial to apply.
The specific embodiment: the preparation process of present embodiment is as follows: the ratio of 1 part of extracting honeysuckle, 2 parts of Fructus Forsythiaes, 1 part of Radix Scutellariae is prepared material by weight, respectively according to following method preparation:
A. the preparation of Fructus Forsythiae: the A-a. Fructus Forsythiae was soaked 20～40 minutes, decocts 2～3 times, and each 1 hour, merging filtrate; A-b. filter, the clear paste of proportion 1.20-1.25 when heating is concentrated into 70-80 ℃ adds the gelatin that accounts for input raw medicinal herbs weight 0.5% again; When A-c. being cooled to 35-40 ℃, slowly add the ethanol that mass concentration is 90%-95%, stir fully simultaneously, make to contain alcohol amount and reach more than 80%, stop to stir; A-d. refrigeration cool-down is incubated cold preservation 24～48 hours to 0-5 ℃; A-e. the leaching supernatant returns alcohol and concentrates, and the distilled water that adds meltage stirs; A-f. be incubated 0-5 ℃ and placed 24～48 hours, leaching supernatant, the clear paste of proportion 1.1-1.15 when heating is concentrated into 70-80 ℃; A-g. be warming up to 35-40 ℃, stir, slowly add the ethanol of mass concentration 94% or more, make to contain the alcohol amount and reach more than 90%, stop stirring; A-h. be chilled to 0-5 ℃, insulation cold preservation 24～48 hours; A-i. the leaching supernatant returns alcohol and concentrates, and the distilled water that adds meltage stirs; A-j. keep temperature 0-5 ℃ to place after 24～48 hours, the leaching supernatant, the clear paste of proportion 1.1-1.15 was Fructus Forsythiae extractum when heating was concentrated into 70-80 ℃, and is standby;
B. the preparation of Flos Lonicerae: the distinctive points of preparation method of Flos Lonicerae and A step is that in the A-b step, the gelatin amount of adding accounts for and drops into 0.6% of raw medicinal herbs weight; Added following process before A-f step, A-j step respectively: " the NaOH solution that slowly adds deployed mass concentration 10% is transferred PH=5, is heated to boiling, is incubated 27～33 minutes; " gains are Flos Lonicerae extractum;
C. the preparation of Radix Scutellariae: C-a. gets Radix Scutellariae section and decocts with water 2-3 time, and each 1 hour, gradation filtration, merging filtrate; C-b. filtrate was regulated pH value to 1.0～2.0 with the hydrochloric acid of 2mol/L, 80 ℃ of insulations 30 minutes; C-c. be chilled to 0-7 ℃ and left standstill 12-48 hour, filter, precipitate adds 8 times of water gagings, stirs; C-d. the sodium hydroxide solution that slowly adds mass concentration 40% is regulated pH value to 7.0; C-e. slowly adding the ethanol of mass concentration more than 95% makes and contains alcohol amount and reach 50%, stirring and dissolving; C-f. filter, filtrate is regulated pH value to 2.0 with the hydrochloric acid of 2mol/L, and 60 ℃ are incubated 30 minutes; C-g. be chilled to 0-5 ℃ and leave standstill more than 12 hours, filter; C-h. to be washed till pH value with the ethanol of mass concentration more than 90% be 4.0 to precipitate, adds the water that accounts for 10 times of amounts of precipitate, stirs; C-i. be that 40% sodium hydroxide solution is regulated pH value to 7.0 with mass concentration; C-j. add active carbon, make active carbon content account for 0.5% of gross weight, fully stir, 50 ℃ are incubated 30 minutes; C-k. slowly adding the ethanol of mass concentration more than 95% makes and contains alcohol amount and reach 50%; C-l. filter immediately after stirring, filtrate is regulated pH value to 2.0 with the hydrochloric acid of 2mol/L, and 60 ℃ are incubated 30 minutes; C-m. be chilled to 0-5 ℃, left standstill 12 hours, filter; C-n. after precipitate was measured 95% washing with alcohol with 1 times, in dry below 60 ℃, it was standby to get baicalin;
Water fully kneads into the suspendible shape with baicalin, NaOH aqueous solution with mass concentration 6% is transferred pH value to 6.0～7.0, with Flos Lonicerae extractum, Fructus Forsythiae extractum and baicalin mix homogeneously, add concentration and transfer PH6.5～7.2 then, add water for the 6%NaOH aqueous solution, boiling sterilization 30 minutes, fill, the freeze dryer of packing into is set to-45 ℃ with the flaggy temperature, 2～3 hours, and then setting flaggy temperature is-10 ℃ of distillations; The distillation time is 25～30 hours, and resetting the flaggy temperature is 50 ℃, 3 hours rear pressing covers, and packing is promptly.
Claims (1)
1. the preparation method of a dual coptis powder injection is characterized in that the ratio of 1 part of extracting honeysuckle, 2 parts of Fructus Forsythiaes, 1 part of Radix Scutellariae is prepared material by weight, respectively according to following method preparation:
A. the preparation of Fructus Forsythiae: the A-a. Fructus Forsythiae was soaked 20～40 minutes, decocts 2～3 times, and each 1 hour, merging filtrate; A-b. filter, the clear paste of proportion 1.20-1.25 when heating is concentrated into 70-80 ℃ adds the gelatin that accounts for input raw medicinal herbs weight 0.5% again; When A-c. being cooled to 35-40 ℃, slowly add the ethanol that mass concentration is 90%-95%, stir fully simultaneously, make to contain alcohol amount and reach more than 80%, stop to stir; A-d. refrigeration cool-down is incubated cold preservation 24～48 hours to 0-5 ℃; A-e. the leaching supernatant returns alcohol and concentrates, and the distilled water that adds meltage stirs; A-f. be incubated 0-5 ℃ and placed 24～48 hours, leaching supernatant, the clear paste of proportion 1.1-1.15 when heating is concentrated into 70-80 ℃; A-g. be warming up to 35-40 ℃, stir, slowly add the ethanol of mass concentration 94% or more, make to contain the alcohol amount and reach more than 90%, stop stirring; A-h. be chilled to 0-5 ℃, insulation cold preservation 24～48 hours; A-i. the leaching supernatant returns alcohol and concentrates, and the distilled water that adds meltage stirs; A-j. keep temperature 0-5 ℃ to place after 24～48 hours, the leaching supernatant, the clear paste of proportion 1.1-1.15 was Fructus Forsythiae extractum when heating was concentrated into 70-80 ℃, and is standby;
B. the preparation of Flos Lonicerae: the distinctive points of preparation method of Flos Lonicerae and A step is that in the A-b step, the gelatin amount of adding accounts for and drops into 0.6% of raw medicinal herbs weight; Added following process before A-f step, A-j step respectively: " the NaOH solution that slowly adds deployed mass concentration 10% is transferred PH=5, is heated to boiling, is incubated 27～33 minutes; " gains are Flos Lonicerae extractum;
C. the preparation of Radix Scutellariae: C-a. gets Radix Scutellariae section and decocts with water 2-3 time, and each 1 hour, gradation filtration, merging filtrate; C-b. filtrate was regulated pH value to 1.0～2.0 with the hydrochloric acid of 2mol/L, 80 ℃ of insulations 30 minutes; C-c. be chilled to 0-7 ℃ and left standstill 12-48 hour, filter, precipitate adds 8 times of water gagings, stirs; C-d. the sodium hydroxide solution that slowly adds mass concentration 40% is regulated pH value to 7.0; C-e. slowly adding the ethanol of mass concentration more than 95% makes and contains alcohol amount and reach 50%, stirring and dissolving; C-f. filter, filtrate is regulated pH value to 2.0 with the hydrochloric acid of 2mol/L, and 60 ℃ are incubated 30 minutes; C-g. be chilled to 0-5 ℃ and leave standstill more than 12 hours, filter; C-h. to be washed till pH value with the ethanol of mass concentration more than 90% be 4.0 to precipitate, adds the water that accounts for 10 times of amounts of precipitate, stirs; C-i. be that 40% sodium hydroxide solution is regulated pH value to 7.0 with mass concentration; C-j. add active carbon, make active carbon content account for 0.5% of gross weight, fully stir, 50 ℃ are incubated 30 minutes; C-k. slowly adding the ethanol of mass concentration more than 95% makes and contains alcohol amount and reach 50%; C-1. filter immediately after stirring, filtrate is regulated pH value to 2.0 with the hydrochloric acid of 2mol/L, and 60 ℃ are incubated 30 minutes; C-m. be chilled to 0-5 ℃, left standstill 12 hours, filter; C-n. after precipitate was measured 95% washing with alcohol with 1 times, in dry below 60 ℃, it was standby to get baicalin;
Water fully kneads into the suspendible shape with baicalin, NaOH aqueous solution with mass concentration 6% is transferred pH value to 6.0～7.0, with Flos Lonicerae extractum, Fructus Forsythiae extractum and baicalin mix homogeneously, add concentration and transfer PH 6.5～7.2 then, add water for the 6%NaOH aqueous solution, boiling sterilization 30 minutes, fill, the freeze dryer of packing into is set to-45 ℃ with the flaggy temperature, 2～3 hours, and then setting flaggy temperature is-10 ℃ of distillations; The distillation time is 25～30 hours, and resetting the flaggy temperature is 50 ℃, 3 hours rear pressing covers, and packing is promptly.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266386A (en) * | 2010-06-01 | 2011-12-07 | 四川大千药业有限公司 | Scutellaria baicalensis extract and preparation method and uses thereof |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526391A (en) * | 2010-12-16 | 2012-07-04 | 天津中敖生物科技有限公司 | Livestock Chinese medicinal composition with refrigerating function and preparation method thereof |
| CN102935113B (en) * | 2012-12-03 | 2014-10-01 | 哈药集团中药二厂 | Preparation method for Shuanghuanglian granules using fluidized drying granulation |
| CN103405507A (en) * | 2013-07-31 | 2013-11-27 | 哈药集团中药二厂 | Preparation method of shuanghuanglian freeze-dried powder for intravenous injection |
| CN106344663A (en) * | 2016-08-26 | 2017-01-25 | 贵州大学 | Preparation method of Jin Ying Huang Gui injection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266386A (en) * | 2010-06-01 | 2011-12-07 | 四川大千药业有限公司 | Scutellaria baicalensis extract and preparation method and uses thereof |
| CN102266386B (en) * | 2010-06-01 | 2013-05-01 | 四川大千药业有限公司 | Scutellaria baicalensis extract and preparation method and uses thereof |
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