CN101084952B - Method for preparing extraction of acanthopanax senticousus saponins - Google Patents
Method for preparing extraction of acanthopanax senticousus saponins Download PDFInfo
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- CN101084952B CN101084952B CN 200610014210 CN200610014210A CN101084952B CN 101084952 B CN101084952 B CN 101084952B CN 200610014210 CN200610014210 CN 200610014210 CN 200610014210 A CN200610014210 A CN 200610014210A CN 101084952 B CN101084952 B CN 101084952B
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- extraction
- exchange column
- saponins
- basic anion
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Abstract
The invention discloses a process for preparing acanthopanax root saponin extract comprising the following steps in sequence, charging dissolvent into acanthopanax root, rhizome, stem or leaf, adjusting the solution to alkalinity, carrying out extraction, obtaining extract, passing the extract through macroscopic alkaline anion exchange resin, flushing with alkaline water and pure water, discarding the flushing fluid, eluting with water-containing ethanol, and concentrating the eluent.
Description
Technical field
The invention belongs to the preparation method of Chinese medical extract, specifically, relate to the preparation method of extraction of acanthopanax senticousus saponins.
Background technology
Radix Et Caulis Acanthopanacis Senticosi is the dry rhizome of Araliaceae (Radix Acanthopanacis Senticosi), receives the concern of Chinese scholars because of having physiologically active widely.The staple of Radix Et Caulis Acanthopanacis Senticosi is a triterpenoid saponin, and particularly the oleanolic acid saponin(e has now and finds nearly 20 kinds of saponin(es.Radix Et Caulis Acanthopanacis Senticosi total saponins have help strong, replenish qi to invigorate the spleen, strengthen the body resistance to consolidate the constitution, effect such as tranquillizing and allaying excitement, be a kind of immunostimulant, can regulate human body metabolism, enhances human body is to the resistibility of various diseases.For the extraction of Radix Et Caulis Acanthopanacis Senticosi saponin(e, traditional technology is with the Radix Et Caulis Acanthopanacis Senticosi medicine materical crude slice, with the method for water extraction or 75% extraction using alcohol, perhaps after extraction, decolours with macroporous resin.Traditional technology, extraction separation efficient is low, and efficient part or composition purity are not high, and therefore, the extraction and separation method of studying more effective and highly purified Radix Et Caulis Acanthopanacis Senticosi saponin(e has great importance.
Summary of the invention
The object of the present invention is to provide the preparation method of more reasonable, the quality controllable extraction of acanthopanax senticousus saponins of a kind of technology.
The present invention implements through following technical proposals.
The preparation method of extraction of acanthopanax senticousus saponins of the present invention comprises the steps: in order
(1) get Radix Acanthopanacis Senticosi root, rhizome or stem, perhaps Folium Acanthopanacis Senticosi adds solvent, extract again after solution is transferred to alkalescence, extracting solution;
(2) macroporous type basic anion exchange column on the extracting solution, earlier with buck and pure water rinsing, washing fluid discards, and uses the aqueous ethanol wash-out again, and elutriant concentrates, and promptly gets extraction of acanthopanax senticousus saponins.
The said solvent of step (1) is water or aqueous ethanol; Said solution transfers to alkalescence and is adjust pH 9～14, available NaOH or KOH or Na
2CO
3Perhaps NaHCO
3Regulate the pH value.
The further removal of impurities of the said extracting solution of step (1), aqueous extract can be used the alcohol precipitating method removal of impurities, and alcohol extract can be used the removal of impurities of depositing in water method.
The preferred macroporous type weakly-basic anion of step (2) said macroporous type basic anion exchange column D392, D380, D382, D371 exchange column, perhaps macroporous type strongly basic anion D201 exchange column; Buck can be 1～3%NaOH or KOH or Na
2CO
3Said aqueous ethanol is 40～95% ethanol.
Total saponin content in the extraction of acanthopanax senticousus saponins of use the inventive method preparation is 15%～85%, is generally 25%～65%, Radix Et Caulis Acanthopanacis Senticosi total saponins assay reference literature (Chinese patent medicine, in January, 2003,25 (1): 12).Prepared extraction of acanthopanax senticousus saponins can be independent; Perhaps share with other activeconstituentss; The various formulations that are mixed and made into auxiliary material such as starch, dextrin, lactose, Microcrystalline Cellulose, HPMC, polyoxyethylene glycol, Magnesium Stearate, micropowder silica gel, Xylitol, Saccharum lactis, glucose, glycocoll, N.F,USP MANNITOL, glycocoll, hydroxypropyl-beta-cyclodextrin etc. on any or more than one pharmaceuticies; For example, can be made into injection, tablet, slow releasing tablet, dripping pill, granule, powder injection, capsule, microgranules.Preferred dosage form is powder injection, pill, capsule.
Compared with prior art, extraction of acanthopanax senticousus saponins preparing method's of the present invention extraction separation efficient is high, and Radix Et Caulis Acanthopanacis Senticosi total saponins content is high, can keep higher physiologically active.
Embodiment
To be easier to understand the present invention with reference to the following example, and provide embodiment and be in order to illustrate the present invention, rather than in order to limit scope of the present invention.
Embodiment one
Get Radix Et Caulis Acanthopanacis Senticosi medicinal material (root, rhizome, stem); Pulverizing, add water boil and extract three times and control potential of hydrogen, is for the first time the Na2CO3 of the 6 times of water yields and the 0.7% medicinal material amount of medicinal material amount; Being for time the Na2CO3 of the 4 times of water yields and the 0.3% medicinal material amount of medicinal material amount, is 4 times of water yields of medicinal material amount for the third time; The side circulated in countercurrent is extracted, and keeps respectively after boiling 1.5,1,1 hours; Combining medicine is chilled to room temperature, filters, and the macroporous type weakly-basic anion D392 exchange column of having handled well on the filtrating (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, washing fluid discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 70% ethanol elution of 7 times of resin bed volumes, collect elutriant, be concentrated into thick paste (50 ℃ of following specific densities are 1.28～1.33), dry with dynamic belt drying equipment, get manyprickle acanthopanax general saponin extractive (total saponin content 31.6%).
Embodiment two
Get Folium Acanthopanacis Senticosi; Smashing to pieces, add water supersound extraction four times and control potential of hydrogen, for the first time is the NaHCO3 of the 5 times of water yields and the 0.9% medicinal material amount of medicinal material amount; For the second time being the NaHCO3 of the 4 times of water yields and the 0.5% medicinal material amount of medicinal material amount, is 3 times of water yields of medicinal material amount with the 4th time for the third time; Combining medicine is chilled to room temperature, filters, and the macroporous type weakly-basic anion D380 exchange column of having handled well on the soup filtrating (Chemical Plant of Nankai Univ.), with the 2.5%NaOH solution flushing of 1.5 times of resin bed volumes, washing fluid discards; 4 times of pure water rinsing again, aqueous rinse solution discards; With 65% ethanol elution of 8 times of resin bed volumes, collect elutriant, be concentrated into thick paste (50 ℃ of following specific densities are 1.28～1.33), dry with dynamic belt drying equipment, get manyprickle acanthopanax general saponin extractive (total saponin content 35.2%).
Embodiment three
Get Radix Et Caulis Acanthopanacis Senticosi medicinal material (root, rhizome, stem); Pulverize; Add 50% alcohol reflux three times and control potential of hydrogen; For the first time be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medicinal material amount of medicinal material amount, be the Na2CO3 of 4 times of 50% amount of alcohol and the 0.5% medicinal material amount of medicinal material amount the second time, is 4 times of 50% amount of alcohol of medicinal material amount for the third time; Side circulated in countercurrent refluxing extraction kept respectively 1.5,1,1 hours after the beginning that refluxes; Medical filtration and merging filtrate; Filtrate be evaporated under 70 ℃ do not have the alcohol flavor after; Liquid concentrator thin up to medicinal material soup ratio is 1: 1.5, filters the macroporous type strongly basic anion D201 exchange column of having handled well on the filtrating (Chemical Plant of Nankai Univ.); With the 2%NaOH solution flushing of 2 times of resin bed volumes, washing fluid discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 7 times of resin bed volumes, collect elutriant, be concentrated into thick paste (50 ℃ of following specific densities are 1.28～1.33), dry with dynamic belt drying equipment, get manyprickle acanthopanax general saponin extractive (total saponin content 47.3%).
Embodiment four
Get Folium Acanthopanacis Senticosi; Smashing to pieces, add water boil and extract three times and control potential of hydrogen, is for the first time the Na2CO3 of the 6 times of water yields and the 0.7% medicinal material amount of medicinal material amount; For the second time being the Na2CO3 of the 4 times of water yields and the 0.3% medicinal material amount of medicinal material amount, is 4 times of water yields of medicinal material amount for the third time; The side circulated in countercurrent is extracted, and keeps respectively after boiling 1.5,1,1 hours; Combining medicine is chilled to room temperature, and 2 times of volumes of concentrated medicament to medicinal material amount add ethanol and make and contain alcohol amount and reach 70%, leave standstill 24 hours, filter, and decompression filtrate recycling ethanol is dissolved in water to there not being the alcohol flavor, filters; The macroporous type weakly-basic anion D382 exchange column of having handled well on the filtrating (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, washing fluid discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 70% ethanol elution of 7 times of resin bed volumes, collect elutriant, be concentrated into thick paste (50 ℃ of following specific densities are 1.28～1.33), dry with dynamic belt drying equipment, get manyprickle acanthopanax general saponin extractive (total saponin content 64.6%).
Embodiment five
Get Radix Et Caulis Acanthopanacis Senticosi medicinal material (root, rhizome, stem); Pulverize; Add water supersound extraction four times and control potential of hydrogen; For the first time be the NaHCO3 of the 5 times of water yields and the 0.9% medicinal material amount of medicinal material amount, be the NaHCO3 of the 4 times of water yields and the 0.5% medicinal material amount of medicinal material amount the second time, is 3 times of water yields of medicinal material amount with the 4th time for the third time; Combining medicine is chilled to room temperature, and 2 times of volumes of concentrated medicament to medicinal material amount add ethanol and make and contain alcohol amount and reach 80%, leave standstill 24 hours, filter, and decompression filtrate recycling ethanol is dissolved in water to there not being the alcohol flavor, filters; The macroporous type strongly basic anion D201 exchange column of having handled well on the filtrating (Chemical Plant of Nankai Univ.), with the 2.5%NaOH solution flushing of 1.5 times of resin bed volumes, washing fluid discards; 4 times of pure water rinsing again, aqueous rinse solution discards; With 85% ethanol elution of 8 times of resin bed volumes, collect elutriant, be concentrated into thick paste (50 ℃ of following specific densities are 1.28～1.33), dry with dynamic belt drying equipment, get manyprickle acanthopanax general saponin extractive (total saponin content 57.4%).
Embodiment six
Get Folium Acanthopanacis Senticosi; Smash to pieces; Add 70% ethanol ultrasonic extraction three times and control potential of hydrogen; For the first time be the Na2CO3 of 5 times of 70% amount of alcohol and the 1% medicinal material amount of medicinal material amount, be the Na2CO3 of 4 times of 70% amount of alcohol and the 0.5% medicinal material amount of medicinal material amount the second time, is 4 times of 70% amount of alcohol of medicinal material amount for the third time; Combining medicine is chilled to room temperature; Filter, filtrate be evaporated under 70 ℃ do not have alcohol and distinguish the flavor of after, liquid concentrator thin up to medicinal material soup ratio is 1: 1.5; Centrifugal; The macroporous type weakly-basic anion D371 exchange column of having handled well on the supernatant (Chemical Plant of Nankai Univ.), with the 2%NaOH solution flushing of 2 times of resin bed volumes, washing fluid discards; 3 times of pure water rinsing again, aqueous rinse solution discards; With 75% ethanol elution of 7 times of resin bed volumes, collect elutriant, be concentrated into thick paste (50 ℃ of following specific densities are 1.28～1.33), dry with dynamic belt drying equipment, get manyprickle acanthopanax general saponin extractive (total saponin content 61.3%).
Embodiment seven
Get the manyprickle acanthopanax general saponin extractive 110g of embodiment four, mix, add Yelkin TTS and each 195g of N.F,USP MANNITOL, an amount of water for injection; After heating made dissolving, adjust pH to 6.5～7.0 added the injection water to TV; Stirred 10 minutes, be chilled to room temperature after, aseptic filtration; The filtrating can is in cillin bottle, and lyophilize, is added a cover at tamponade, promptly gets.
Embodiment eight
Get the manyprickle acanthopanax general saponin extractive 170g of embodiment three, mix, add 3% polyvidone ethanolic soln system softwood, cross 18 mesh sieve system particles with the 80g Microcrystalline Cellulose; 600 ℃ of dryings 30～45 minutes, whole grain adds the 10g talcum powder; Mixing fills in capsule, promptly gets.
Embodiment nine
Get the manyprickle acanthopanax general saponin extractive 160g of embodiment six, mix with 700g polyoxyethylene glycol-6000, fusion splashes in the cryogenic liquid paraffin, selects ball, removes whiteruss, promptly gets.
The preparation method of extraction of acanthopanax senticousus saponins provided by the invention, most preferably, it comprises the steps: in order
(1) get Radix Acanthopanacis Senticosi root, rhizome or stem, perhaps Folium Acanthopanacis Senticosi adds entry or 40～95% ethanol, and solution is transferred to alkalescence be adjust pH 9～14, heating or supersound extraction 2～4 times, united extraction liquid filters; The further removal of impurities of filtrating, aqueous extract is used the alcohol precipitating method removal of impurities, and alcohol extract is then used the removal of impurities of depositing in water method, obtains the clear liquor after the removal of impurities;
(2) macroporous type weakly-basic anion D392 exchange column, macroporous type weakly-basic anion D380 exchange column, macroporous type weakly-basic anion D382 exchange column, macroporous type weakly-basic anion D371 exchange column or macroporous type strongly basic anion D201 exchange column on the clear liquor are earlier with 1～3%NaOH, 1～3%KOH or 1～3%Na
2CO
3Pure water rinsing is used in flushing again, and washing fluid discards, and uses 40～95% ethanol elutions then, and elutriant concentrates, and drying promptly gets extraction of acanthopanax senticousus saponins.
The preparation method of Radix Et Caulis Acanthopanacis Senticosi saponin(e powder injection provided by the invention most preferably, comprises the steps: to get the extraction of acanthopanax senticousus saponins that obtains according to the method described above; Add Yelkin TTS and N.F,USP MANNITOL and an amount of water for injection, after heating makes dissolving, adjust pH to 6.5～7.0; Add the injection water to specified volume, stir cold putting; Filter, the filtrating lyophilize promptly gets.
Claims (2)
1. the preparation method of an extraction of acanthopanax senticousus saponins is characterized in that, it comprises the steps: in order
(1) get Radix Acanthopanacis Senticosi root, rhizome or stem, perhaps Folium Acanthopanacis Senticosi adds entry or 40～95% ethanol, and solution is transferred to alkalescence be adjust pH 9～14, heating or supersound extraction 2～4 times, united extraction liquid filters; The further removal of impurities of filtrating, aqueous extract is used the alcohol precipitating method removal of impurities, and alcohol extract is then used the removal of impurities of depositing in water method, obtains the clear liquor after the removal of impurities;
(2) macroporous type weakly-basic anion D392 exchange column, macroporous type weakly-basic anion D380 exchange column, macroporous type weakly-basic anion D382 exchange column, macroporous type weakly-basic anion D371 exchange column or macroporous type strongly basic anion D201 exchange column on the clear liquor are earlier with 1～3%NaOH, 1～3%KOH or 1～3%Na
2CO
3Pure water rinsing is used in flushing again, and washing fluid discards, and uses 40～95% ethanol elutions then, and elutriant concentrates, and drying promptly gets extraction of acanthopanax senticousus saponins.
2. the preparation method of a Radix Et Caulis Acanthopanacis Senticosi saponin(e powder injection comprises the steps: the extraction of acanthopanax senticousus saponins that the weighting profit requires 1 said method to obtain, and adds Yelkin TTS and N.F,USP MANNITOL and an amount of water for injection; After heating made dissolving, adjust pH to 6.5～7.0 added the injection water to specified volume; Stir, cold putting filters; The filtrating lyophilize promptly gets.
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| CN 200610014210 CN101084952B (en) | 2006-06-08 | 2006-06-08 | Method for preparing extraction of acanthopanax senticousus saponins |
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| CN 200610014210 CN101084952B (en) | 2006-06-08 | 2006-06-08 | Method for preparing extraction of acanthopanax senticousus saponins |
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| CN101084952B true CN101084952B (en) | 2012-03-14 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584719B (en) * | 2008-05-20 | 2011-11-09 | 李平亚 | Application of acanthopanax fruit extractive in preparing medicament for treating hyperlipoidemia |
| CN102488764B (en) * | 2011-12-29 | 2013-10-16 | 中国人民解放军第三军医大学第一附属医院 | Preparation method for total saponins of Rubus parviflolius |
| CN102512506A (en) * | 2012-01-01 | 2012-06-27 | 山东大学威海分校 | Compound acanthopanax root preparation capable of improving activity of superoxide dismutase |
| CN102579531A (en) * | 2012-02-20 | 2012-07-18 | 山东大学威海分校 | Acanthopanax leaf extract having antioxidation |
| CN103859520B (en) * | 2014-04-03 | 2015-08-26 | 通化师范学院 | Contribute to acanthopanax fruit oral liquid and the preparation method of improving water flood function |
| CN111374993A (en) * | 2018-12-29 | 2020-07-07 | 华北理工大学 | Method for extracting acanthopanax senticosus total saponin from acanthopanax senticosus leaves |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176671C (en) * | 2000-09-29 | 2004-11-24 | 哈药集团中药二厂 | Productive technology for producing Jiatong powder injection |
| CN1206236C (en) * | 2002-07-19 | 2005-06-15 | 哈尔滨誉衡药业有限公司 | Manyprickle acanthopanax general saponin extractive and its medicinal composition |
| CN1285344C (en) * | 2003-12-27 | 2006-11-22 | 天津天士力之骄药业有限公司 | Method for preparing acanthopanax injectio |
-
2006
- 2006-06-08 CN CN 200610014210 patent/CN101084952B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176671C (en) * | 2000-09-29 | 2004-11-24 | 哈药集团中药二厂 | Productive technology for producing Jiatong powder injection |
| CN1206236C (en) * | 2002-07-19 | 2005-06-15 | 哈尔滨誉衡药业有限公司 | Manyprickle acanthopanax general saponin extractive and its medicinal composition |
| CN1285344C (en) * | 2003-12-27 | 2006-11-22 | 天津天士力之骄药业有限公司 | Method for preparing acanthopanax injectio |
Non-Patent Citations (2)
| Title |
|---|
| 施海平.大孔吸附树脂法在刺五加提取工艺中的应用.《哈尔滨医药》.2004,第24卷(第6期),44-45. * |
| 李庆勇.刺五加有效成分的提取_纯化及利用.《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》.2002,(第1期),29. * |
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