CN100369611C - Method for preparing freeze dried acanthopanax injectio - Google Patents
Method for preparing freeze dried acanthopanax injectio Download PDFInfo
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- CN100369611C CN100369611C CNB200410043998XA CN200410043998A CN100369611C CN 100369611 C CN100369611 C CN 100369611C CN B200410043998X A CNB200410043998X A CN B200410043998XA CN 200410043998 A CN200410043998 A CN 200410043998A CN 100369611 C CN100369611 C CN 100369611C
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Abstract
The present invention relates to a preparation method of an acanthopanax freeze drying powder injection solution used for injection. The production method of the existing acanthopanax freeze drying injection solution used for injection has the defects of low purity and low content of effective components. The preparation process of the preparation method of the acanthopanax freeze drying powder injection solution used for injection comprises the following steps: a. roots, rootstocks or stems of the acanthopanax is extracted by water or by alcohol; b. precipitation is carried out for more than 24 hours, and the alcohol is recovered and refrigerated for 24 hours after being added with water; c. adsorption is carried out by macroporous adsorption resin, and than, the adsorption resin is eluted by the alcohol, alcohol eluting liquid is recovered and alcohol is recovered until no alcohol taste exists; d. refrigeration and filtration by watering, sterilization, sterile subpackage, freeze drying and package are carried out. The preparation method of the present invention has the advantages of simple process and easy operation; the main components of medicine prepared by the method is clear; the present invention is suitable for industrial production, and is beneficial to popularization and application.
Description
Technical field:
The present invention relates to a kind of production method of injection Radix Et Caulis Acanthopanacis Senticosi freeze-dried powder.
Background technology:
There is the drawback that purity is low, active constituent content is low in the production method of existing injection Radix Et Caulis Acanthopanacis Senticosi freeze-dried powder.ZL94107718.7 discloses a kind of " Radix Et Caulis Acanthopanacis Senticosi extract and production technology thereof and the injection and the lyophilized injectable powder that contain this extract ", this patent has adopted the macroporous adsorbent resin decolouring in preparation process, with ethyl acetate extraction, will extract back liquid and processes such as destaining solution mixes, because extraction process can reduce the recovery of effective ingredient, and it is single to reclaim composition, and ethyl acetate toxicity is big, belong to combustibles again, can cause great injury to human body, its appropriate experimental chamber research is not suitable for suitability for industrialized production; And, steaming excess after this patent in the end will extract mixes with destaining solution, because destaining solution belongs to saccharide, micromolecule class, its impurity is very many, this mixing meeting reduces the purity of medicine greatly, reduce the content of effective ingredient, so in actual applications, the medicine that obtains with this method has the bad drawback of curative effect.
Summary of the invention:
The object of the present invention is to provide simple, the workable and effective ingredient gained medicine of a kind of production process to keep the preparation method of injection Radix Et Caulis Acanthopanacis Senticosi lyophilized injectable powder completely, its preparation process comprises the steps: that a. proposes root, rhizome or the stem water of Radix Et Caulis Acanthopanacis Senticosi or alcohol extraction, makes to contain alcohol amount and reach 80～88%; B. precipitate more than 24 hours, reclaim ethanol, add water-cooled again and hid 24 hours; C. use absorption with macroporous adsorbent resin, use the ethanol elution adsorbent resin then, reclaim eluting ethanol liquid, reclaim ethanol to there not being the alcohol flavor, detailed process is as follows: filtrate is joined in the macroporous adsorptive resins, flow velocity with 1500～4000ml/s flows out, impurity on elder generation's water flush away adsorption resin column, the reuse mass concentration is 80～85% ethanol elution, used amount of alcohol is 3～6 times of weight resin, collect ethanol elution, reclaim ethanol to not having alcohol flavor, the clear paste of relative density 1.10～1.15 when then gains being concentrated into 80 ℃; D. add water-cooled and hide filtration, sterilization, aseptic subpackaged, lyophilizing, packing gets final product.The present invention's purpose with absorption with macroporous adsorbent resin in the preparation of product process is not decolouring, but in order to adsorb the effective ingredient of medicine; The present invention does not mix adsorbate in the preparation process of product with effluent, but the effluent that will contain high impurity gives up, and the purity of products obtained therefrom is improved; The present invention gives up this process of usefulness ethyl acetate extraction in the prior art, can make main component ligustrin, the isofraxidin of medicine be able to abundant reservation like this, and the active constituent content of products obtained therefrom is improved; Preparation method of the present invention has simple, the maneuverable advantage of technology, and with the drug main definite ingredients of this method preparation, suitability for industrialized production is beneficial to and applies.
The specific embodiment:
The specific embodiment one: the preparation process of present embodiment comprises the steps: that a. proposes root, rhizome or the stem water of Radix Et Caulis Acanthopanacis Senticosi or alcohol extraction, makes to contain alcohol amount and reach 80～88%; B. precipitate more than 24 hours, reclaim ethanol, add water-cooled again and hid 24 hours; C. use absorption with macroporous adsorbent resin, use the ethanol elution adsorbent resin then, reclaim eluting ethanol liquid, reclaim ethanol to there not being the alcohol flavor; D. add water-cooled and hide filtration, sterilization, aseptic subpackaged, lyophilizing, packing gets final product.
The specific embodiment two: the preparation process of present embodiment is as follows: get Caulis Et Caulis Acanthopanacis Senticosi powder (sheet or section) or root powder (sheet or section) 40000g-50000g, decoct with water three times, each 2 hours, amount of water is 8 times of amount to 10 times amounts, gradation filters, merging filtrate, filtrate decompression is concentrated into the clear paste that relative density is 1.10-1.15 (80 ℃ of survey), adding ethanol makes the alcohol amount of containing reach 75%-88%, left standstill 24 hours, filter, filtrate recycling ethanol also is concentrated into the extractum of relative density 1.20-1.25 (80 ℃ of surveys), adding 2-3 doubly hid 24 hours to the water-cooled of crude drug amount, filter, filtrate is joined in the macroporous adsorptive resins, used adsorbent resin model is the AB-8 type, flow velocity with 1500～4000ml/s flows out then, the impurity on the first water flush away adsorption resin column, and the reuse mass concentration is 80～85% ethanol elution, used amount of alcohol is 3～6 times of weight resin, collect ethanol elution, reclaim ethanol to not having alcohol flavor, the clear paste of relative density 1.10～1.15 when then gains being concentrated into 80 ℃, put cold, the purified water or the water for injection that add 4～5 times of amounts again, cold preservation 24 hours filters, filtrate adds water to full dose, regulate pH value to 7.0～7.8, filter sterilization, packing, lyophilization, pre-freeze temperature-30 ℃, sublimation temperature≤-8 ℃, vacuum 0.1mmg; 30 ℃～35 ℃ of later stage baking temperatures, total sublimation drying 30～40 hours freezes altogether and makes 1000 injection Radix Et Caulis Acanthopanacis Senticosi powder pins.
Above-mentioned whole technical process quality control adopts senior liquid phase instrument control, and the preparation finger printing, and production process is simple, and is workable, is applicable to suitability for industrialized production.Through check, in 1000 Radix Et Caulis Acanthopanacis Senticosi injectable powder of said process gained, every contains syringoside (C
17H
24O
9) at 2.5mg～4.0mg, every contain Radix Et Caulis Acanthopanacis Senticosi total glucosides in syringoside at 60～80mg, every contains isofraxidin (C
11H
10O
3) 0.05mg～2.0mg, every contains dry matter weight is 200mg～600mg.
The specific embodiment three: present embodiment is got Radix Et Caulis Acanthopanacis Senticosi rhizome powder (or section or cutting) 40000g～50000g, add 75%～88% alcohol reflux 3 times, each 2～3 hours, adding amount of alcohol is 8～10 times, and gradation filters, and leaves standstill 24 hours, filter, filtrate recycling ethanol also is concentrated into the extractum of relative density 1.20～1.25 (80 ℃ of surveys), adds 2～3 times to the purified water or the water for injection of crude drug amount, cold preservation 24 hours, filter immersion and be added on macroporous adsorptive resins, the big pore adsorption resin model is AB-8, after adsorbing, and first water eluting, the reuse mass concentration is 80%～85% ethanol elution, collect ethanol elution, reclaim ethanol and be concentrated into the clear paste of relative density 1.10-1.15 (80 ℃ of surveys), put cold, the water for injection that adds 4～5 times of amounts, cold preservation 24 hours filters, and filtrate adds to the full amount of water for injection, regulate pH value to 7.0～7.8, filter sterilization, packing, lyophilization.Aforementioned pre-freeze temperature is-30 ℃, sublimation temperature≤-8 ℃, vacuum 0.1mmg.30 ℃～35 ℃ of later stage baking temperatures, total sublimation drying 30～40 hours is made 1000 injection Radix Et Caulis Acanthopanacis Senticosi powder pins altogether.
Above-mentioned whole technical process quality control adopts senior liquid phase instrument control, and the preparation finger printing, and production process is simple, and is workable, is applicable to suitability for industrialized production.Through check, in 1000 Radix Et Caulis Acanthopanacis Senticosi injectable powder of said process gained, every contains syringoside (C
17H
24O
9) at 2.5mg～4.0mg, every contain Radix Et Caulis Acanthopanacis Senticosi total glucosides in syringoside at 60～80mg, every contains isofraxidin (C
11H
10O
3) 0.05mg～2.0mg, every contains dry matter weight is 200mg～600mg.
Claims (3)
1. the preparation method of an injection Radix Et Caulis Acanthopanacis Senticosi lyophilized injectable powder is characterized in that its preparation process comprises the steps: that a. proposes root, rhizome or the stem water of Radix Et Caulis Acanthopanacis Senticosi or alcohol extraction, makes to contain alcohol amount and reach 80～88%; B. precipitate more than 24 hours, reclaim ethanol, add water-cooled again and hid 24 hours; C. use absorption with macroporous adsorbent resin, use the ethanol elution adsorbent resin then, reclaim eluting ethanol liquid, reclaim ethanol to there not being the alcohol flavor, detailed process is as follows: filtrate is joined in the macroporous adsorptive resins, flow velocity with 1500～4000ml/s flows out, impurity on elder generation's water flush away adsorption resin column, the reuse mass concentration is 80～85% ethanol elution, used amount of alcohol is 3～6 times of weight resin, collect ethanol elution, reclaim ethanol to not having alcohol flavor, the clear paste of relative density 1.10～1.15 when then gains being concentrated into 80 ℃; D. add water-cooled and hide filtration, sterilization, aseptic subpackaged, lyophilizing, packing gets final product.
2. the preparation method of a kind of injection Radix Et Caulis Acanthopanacis Senticosi lyophilized injectable powder according to claim 1, the process that it is characterized in that the d step is as follows: add the purified water or the water for injection of 4～5 times of amounts, cold preservation 24 hours filters, filtrate adds water to full dose, regulate pH value to 7.0～7.8, filter sterilization, packing, lyophilization, pre-freeze temperature-30 ℃, sublimation temperature≤-8 ℃, vacuum 0.1mmg; 30 ℃～35 ℃ of later stage baking temperatures, total sublimation drying 30～40 hours.
3. the preparation method of a kind of injection Radix Et Caulis Acanthopanacis Senticosi lyophilized injectable powder according to claim 1 and 2 is characterized in that described macroporous adsorbent resin model is an AB-8 type resin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410043998XA CN100369611C (en) | 2004-10-29 | 2004-10-29 | Method for preparing freeze dried acanthopanax injectio |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410043998XA CN100369611C (en) | 2004-10-29 | 2004-10-29 | Method for preparing freeze dried acanthopanax injectio |
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|---|---|
| CN1634274A CN1634274A (en) | 2005-07-06 |
| CN100369611C true CN100369611C (en) | 2008-02-20 |
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|---|---|---|---|
| CNB200410043998XA Active CN100369611C (en) | 2004-10-29 | 2004-10-29 | Method for preparing freeze dried acanthopanax injectio |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101554370B (en) * | 2008-04-08 | 2011-11-23 | 苑立超 | Syringin for injection, preparation method and application thereof |
| CN102600221A (en) * | 2012-04-20 | 2012-07-25 | 苏州大学 | Preparation method of acanthopanax root extract |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1345592A (en) * | 2000-09-29 | 2002-04-24 | 哈药集团中药二厂 | Productive technology for producing Jiatong powder injection |
| CN1450060A (en) * | 2002-04-10 | 2003-10-22 | 东北林业大学 | Method for producing isoforaxidin, eleutheroside and eleutheran from Radix Acanthopanacis senticosi |
-
2004
- 2004-10-29 CN CNB200410043998XA patent/CN100369611C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1345592A (en) * | 2000-09-29 | 2002-04-24 | 哈药集团中药二厂 | Productive technology for producing Jiatong powder injection |
| CN1450060A (en) * | 2002-04-10 | 2003-10-22 | 东北林业大学 | Method for producing isoforaxidin, eleutheroside and eleutheran from Radix Acanthopanacis senticosi |
Non-Patent Citations (1)
| Title |
|---|
| 高效液相色谱-质谱联用技术分析刺五加抗疲劳化学成分. 王子灿，；乔善义；，马安德；等.第一军医大学学报,，第4卷第23期. 2003 * |
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| CN1634274A (en) | 2005-07-06 |
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Address after: Jixi City, Heilongjiang Province, Mishan City, the town of Pei Patentee after: Heilongjiang Wandashan pharmaceutical Limited by Share Ltd Address before: Jixi City, Heilongjiang Province, Mishan City, the town of Pei Patentee before: Heilongjiang WanDaShan Pharmaceutical Factory |
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Inventor after: Zhang Qingbo Inventor after: Zhang Meng Inventor after: Jiang Bin Inventor after: Bai Junchang Inventor after: Hu Weiliang Inventor after: Liao Hong Inventor after: Wang Yanwei Inventor after: Zhou Hongjin Inventor after: Xing Yintian Inventor after: Shi Haiping Inventor after: Xu Lihua Inventor after: Shi Shili Inventor after: Gong Lijun Inventor after: Jiang Ying Inventor after: Li Weijun Inventor after: Qiu Youhong Inventor before: Zhang Qingbo Inventor before: Zhang Meng Inventor before: Jiang Bin Inventor before: Xing Yintian Inventor before: Shi Haiping Inventor before: Xu Lihua Inventor before: Shi Shili Inventor before: Gong Lijun Inventor before: Jiang Ying Inventor before: Li Weijun Inventor before: Qiu Youhong |
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Address after: 158300 Jixi City, Heilongjiang city in Mishan Province town of Pei Patentee after: HEILONGJIANG JINJIU PHARMACEUTICAL CO., LTD. Address before: 158300 Jixi City, Heilongjiang city in Mishan Province town of Pei Patentee before: Heilongjiang Wandashan pharmaceutical Limited by Share Ltd |