CN103110689A - Novel method for extracting astragaloside from radix astragali - Google Patents
Novel method for extracting astragaloside from radix astragali Download PDFInfo
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- CN103110689A CN103110689A CN 201210595622 CN201210595622A CN103110689A CN 103110689 A CN103110689 A CN 103110689A CN 201210595622 CN201210595622 CN 201210595622 CN 201210595622 A CN201210595622 A CN 201210595622A CN 103110689 A CN103110689 A CN 103110689A
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- radix astragali
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Abstract
The invention aims at overcoming the defects of relatively low extraction rate, low extraction purity and the like in the prior art, and provides a method for enriching and purifying astragaloside contained in radix astragali by utilizing a water vapor reflux extraction and membrane separation technology and a macroporous adsorption resin coupling method. The method provided by the invention can be used for separating and purifying the astragaloside by adopting the water vapor reflux extraction and membrane separation technology and the macroporous adsorption resin coupling method, has the advantages of complete astragaloside extraction without pollution, good separation effect, high purity and good adsorption selectivity, fast absorption, fast resolution, large adsorption capacity, obvious separation effect and high extraction purity of macroporous resin and can obtain the astragaloside semi-finished products with content more than 30% and astragaloside finished products with content more than 95% and overcome the defects of relatively low conventional extraction rate and low extraction purity.
Description
Technical field:
The invention belongs to the natural organic chemistry field, relate to a kind of purification process of Radix Astragali saponin, particularly relate to a kind of method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali.
Background technology:
The Radix Astragali: have another name called Radix Astragali, be the general designation of plant and Chinese crude drug.The plant Radix Astragali originates in the ground such as the Inner Mongol, Shanxi, Gansu, Heilungkiang, is state three level protecting plant.The Chinese crude drug Radix Astragali is the root of leguminous herbaceous plant's Radix Astagali, Radix Astragali, has the effects such as invigorating QI to consolidate the body surface resistance, diuretic detumescent, expelling pus and toxin by strengthening QI, granulation promoting.The medicinal history of existing more than 2000 year so far of the Radix Astragali, modern study, the Radix Astragali contain the various trace elements such as Saponin, sucrose, polysaccharide, several amino acids, folic acid and selenium, zinc, copper.The enhancing human body immunity function arranged, protect the liver, diuresis, defying age, anti-stress, blood pressure lowering and antibacterial action more widely.But the table excess pathogen is contained, the wet sun of the stagnation of QI, food stagnation is stagnated, carbuncle from the beginning of or burst after the excess syndrome such as pyretic toxicity Shang Sheng, and hyperactivity of YANG due to deficiency of YIN person must prohibit clothes.
Radix Astragali saponin is a kind of natural active matter that human health is had remarkable health-care effect, has caused the common concern of international community.Prove through scientific research and clinical practice, Radix Astragali saponin is regulated body's immunity, and the bone marrow hematogenesis of promotion function is arranged, and makes the eugonic effect of bone marrow, and metabolism is significantly improved to the excess of the kidney cell plastid.In recent years, it is found that and contain a large amount of Radix Astragali saponins in the natural plants Radix Astragali, because its raw material Radix Astragali is Chinese medicine, originate wider, therefrom extract Radix Astragali saponin and obtained encouraging progress.Name is called and just discloses in the patent application of " preparation method of Radix Astragali total saponins " Radix Astragali desaccharide after water extraction resin absorption Radix Astragali saponin technological process of decolouring to get.Extracting Process for Radix Astragali in above-mentioned patent documentation is mainly to extract through steps such as water extraction, desaccharide, decolouring purification to form, and its complex process and separating effect are nothing like the effect of carrying out silica gel column chromatography and separate after utilizing water vapour reflux, extract, and membrane separation technique and macroporous adsorbent resin coupled method to process.
Summary of the invention:
The object of the invention is to overcome the shortcomings such as the routine techniques extraction ratio is relatively low, DNA purity is low, a kind of method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali is provided.
For achieving the above object, the technical solution used in the present invention is:
A kind of method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali, its step is as follows:
(1) the dried Radix Astragali is pulverized, adding volume is the purified water of 10～20 times that the Radix Astragali is pulverized volume, carries out the water vapour reflux, extract,, extracts 2～3 hours extraction times 2～3 times;
(2) Radix Astragali extractive solution after process (1) is merged, through microfiltration, pore diameter range is at 0.1～1 micron, and pressure is controlled at 01～0.7MPa, gets filtrate;
(3) will pass through ultrafiltration through the filtrate of microfiltration, temperature is controlled at 20～40 ℃ again, and pressure is controlled at 0.1～0.6MPa, gets the Radix Astragali saponin crude extract;
(4) gained Radix Astragali saponin crude extract employment macroporous adsorbent resin is adsorbed, be adsorbed as static adsorption or dynamic adsorption;
(5) ethanol with 40%～80% variable concentrations carries out eluting to macroporous adsorbent resin, follows the tracks of with thin layer chromatography and detects, and collects each stepwise elution liquid of Radix Astragali saponin;
(6) each stepwise elution liquid of Radix Astragali saponin is concentrated, reclaim ethanol, get the Radix Astragali saponin semi-finished product, its content is more than 30%;
(7) with silica gel column chromatography on gained Radix Astragali saponin semi-finished product, and take the volume ratio of methanol and concentrated solution as 1～7: 1 ratio is carried out eluting, and thin layer chromatography is followed the tracks of and detected, and collects each stepwise elution liquid of Radix Astragali saponin;
(8) with collected Radix Astragali saponin eluent, adopt activated carbon decolorizing, recrystallization method to make with extra care to get Radix Astragali saponin, its content is more than 95%.
In described step (1), after pulverizing, the dried Radix Astragali crosses 40～80 mesh sieves.
In described step (4), macroporous adsorbent resin used is a kind of in Tianjin Nankai university X-5, the NKA-9, S-8, D3520, D4006, H103, D4020, AB-8H and the NKA-II type resin that produce.
The present invention uses water vapour reflux, extract, and membrane separation technique and macroporous adsorbent resin coupled method Seperation Purification of Astragaloside, Radix Astragali saponin is extracted fully, do not pollute, good separating effect, purity is high, the macroporous resin adsorption selectivity is good, the fast parsing of absorption is also fast, adsorption capacity is larger, separating effect is obvious, DNA purity is high, can obtain Radix Astragali saponin semi-finished product and the content Radix Astragali saponin finished product 95% or more of content more than 30%, has overcome the shortcoming that conventional extraction ratio is relatively low, DNA purity is low.
The specific embodiment:
Embodiment 1: a kind of method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali, and its step is as follows:
(1) the dried Radix Astragali of 100g is pulverized rear 60 mesh sieves of crossing, adding volume is the purified water of 10 times that the Radix Astragali is pulverized volume, carries out the water vapour reflux, extract,, extracts 2 hours extraction times 2 times;
(2) Radix Astragali extractive solution after process (1) is merged, through microfiltration, pore diameter range is at 0.1～1 micron, and pressure is controlled at 0.1MPa, gets filtrate;
(3) will pass through ultrafiltration through the filtrate of microfiltration, the ultrafiltration molecular cut off is 3000～300000 again, and temperature is controlled at 20 ℃, and pressure is controlled at 0.1MPa, gets the Radix Astragali saponin crude extract;
(4) gained Radix Astragali saponin crude extract is adsorbed with macroporous adsorbent resin, macroporous resin used is the NKA-II type resin that Tianjin Nankai university produces, and is adsorbed as static adsorption or dynamic adsorption;
(5) carry out successively gradient elution with the ethanol with 40%, 50%, 60%, 70%, 80% in macroporous adsorbent resin layer post, follow the tracks of with thin layer chromatography and detect, collect each stepwise elution liquid of Radix Astragali saponin;
(6) with the standby stepwise elution liquid concentration and recovery ethanol of Radix Astragali saponin, obtaining content is 306% Radix Astragali saponin semi-finished product;
(7) with silica gel column chromatography on gained Radix Astragali saponin semi-finished product, and be followed successively by 1: 1, carried out gradient elution in 2: 1,3: 1,4: 1,5: 1,6: 1,7: 1 with the volume ratio of methanol and concentrated solution, thin layer chromatography is followed the tracks of and is detected, and collects each stepwise elution liquid of Radix Astragali saponin:
(8) with collected Radix Astragali saponin eluent, adopt activated carbon decolorizing, refining content 95.4% Radix Astragali saponin that obtains of recrystallization method
Case study on implementation 2: a kind of method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali, its step is as follows:
(1) the dried Radix Astragali of 100g is pulverized rear 40 mesh sieves of crossing, adding volume is the purified water of 15 times that the Radix Astragali is pulverized volume, carries out the water vapour reflux, extract,, extracts 2 hours extraction times 2 times;
(2) Radix Astragali extractive solution after process (1) is merged, through microfiltration, pore diameter range is at 0.1～1 micron, and pressure is controlled at 0.2MPa, gets filtrate;
(3) will stand through super through the filtrate of microfiltration, the ultrafiltration molecular cut off is 3000～300000 again, and temperature is controlled at 30 ℃, and pressure is controlled at 0.2MPa, gets the Radix Astragali saponin crude extract;
(4) gained Radix Astragali saponin crude extract is adsorbed with macroporous adsorbent resin, macroporous resin used is the D4006 type resin that Tianjin Nankai university produces, and is adsorbed as static adsorption or dynamic adsorption;
(5) carry out successively gradient elution with 40%, 50%, 60%, 70%, 80% ethanol in macroporous adsorbent resin layer post, follow the tracks of with thin layer chromatography and detect, collect each stepwise elution liquid of Radix Astragali saponin;
(6) with each stepwise elution liquid concentration and recovery ethanol of Radix Astragali saponin, obtain content and be 31.2% Radix Astragali saponin semi-finished product;
(7) with silica gel column chromatography on gained Radix Astragali saponin semi-finished product, and be followed successively by 1: 1, carried out gradient elution in 2: 1,3: 1,4: 1,5: 1,6: 1,7: 1 with the volume ratio of methanol and concentrated solution, thin layer chromatography is followed the tracks of and is detected, and collects each stepwise elution liquid of Radix Astragali saponin;
(8) with collected Radix Astragali saponin eluent, adopt activated carbon decolorizing, the refining Radix Astragali saponin that obtains content 96.6% of recrystallization method.
Case study on implementation 3: a kind of method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali, its step is as follows:
(1) the dried Radix Astragali of 100g is pulverized rear 80 mesh sieves of crossing, adding volume is the purified water of 20 times that the Radix Astragali is pulverized volume, carries out the water vapour reflux, extract,, extracts 2 hours extraction times 3 times;
(2) Radix Astragali extractive solution after process (1) is merged, through microfiltration, pore diameter range is at 0.1～1 micron, and pressure is controlled at 0.2MPa, gets filtrate;
(3) will pass through ultrafiltration through the filtrate of microfiltration, the ultrafiltration molecular cut off is 3000～300000 again, and temperature is controlled at 40 ℃, and pressure is controlled at 0.2MPa, gets the Radix Astragali saponin crude extract;
(4) gained Radix Astragali saponin crude extract is adsorbed with macroporous adsorbent resin, macroporous resin used is the NKA-9 type resin that Tianjin Nankai university produces, and is adsorbed as static adsorption or dynamic adsorption;
(5) carry out successively gradient elution with 40%, 50%, 60%, 70%, 80% ethanol in macroporous adsorbent resin layer post, follow the tracks of with thin layer chromatography and detect, collect each stepwise elution liquid of Radix Astragali saponin;
(6) with each stepwise elution liquid concentration and recovery ethanol of Radix Astragali saponin, obtain content and be 31.7% Radix Astragali saponin semi-finished product;
(7) with silica gel column chromatography on gained Radix Astragali saponin semi-finished product, and be followed successively by 1: 1, carried out gradient elution in 2: 1,3: 1,4: 1,5: 1,6: 1,7: 1 with the volume ratio of methanol and concentrated solution, thin layer chromatography is followed the tracks of and is detected, and collects each stepwise elution liquid of Radix Astragali saponin;
(8) with collected Radix Astragali saponin eluent, adopt activated carbon decolorizing, the refining Radix Astragali saponin that obtains content 97.8% of recrystallization method.
Case study on implementation 4: a kind of method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and people's macroporous adsorbent resin coupled method enriching and purifying Radix Astragali, its step is as follows:
(1) the dried Radix Astragali of 100g is pulverized rear 50 mesh sieves of crossing, adding volume is the purified water of 12 times that the Radix Astragali is pulverized volume, carries out the water vapour reflux, extract,, extracts 2 hours extraction times 3 times;
(2) Radix Astragali extractive solution after process (1) is merged, through microfiltration, pore diameter range is at 0.1～1 micron, and pressure is controlled at 0.4MPa, gets filtrate;
(3) will stand through super through the filtrate of microfiltration, the ultrafiltration molecular cut off is 3000～300000 again, and temperature is controlled at 20 ℃, and pressure is controlled at 0.4MPa, gets the Radix Astragali saponin crude extract;
(4) gained Radix Astragali saponin crude extract is adsorbed with macroporous adsorbent resin, macroporous resin used is the H103 type resin that Tianjin Nankai university produces, and is adsorbed as static adsorption or dynamic adsorption;
(5) carry out successively gradient elution with 40%, 50%, 60%, 70%, 80% ethanol in macroporous adsorbent resin layer post, follow the tracks of with thin layer chromatography and detect, collect each stepwise elution liquid of Radix Astragali saponin;
(6) with each stepwise elution liquid concentration and recovery ethanol of Radix Astragali saponin, obtain content and be 30.4% Radix Astragali saponin semi-finished product;
(7) with silica gel column chromatography on gained Radix Astragali saponin semi-finished product, and be followed successively by 1: 1, carried out gradient elution in 2: 1,3: 1,4: 1,5: 1,6: 1,7: 1 with the volume ratio of methanol and concentrated solution, thin layer chromatography is followed the tracks of and is detected, and collects each stepwise elution liquid of Radix Astragali saponin:
(8) with collected Radix Astragali saponin eluent, adopt activated carbon decolorizing, the refining Radix Astragali saponin that obtains content 90.9% of recrystallization method.
Claims (5)
1. method of utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali, its step is as follows:
(1) the dried Radix Astragali is pulverized, added purified water, carry out the water vapour reflux, extract,, extract 2～3 hours extraction times 2～3 times;
(2) Radix Astragali extractive solution after process (1) is merged, through microfiltration, pore diameter range is at 0.1～1 micron, and pressure is controlled at 0.1～07MPa, gets filtrate;
(3) will pass through ultrafiltration through the filtrate of microfiltration, temperature is controlled at 20～40 ℃ again, and pressure is controlled at 01～0.6MPa, gets the Radix Astragali saponin crude extract;
(4) gained Radix Astragali saponin crude extract is adsorbed with macroporous adsorbent resin, be adsorbed as static adsorption or dynamic adsorption;
(5) ethanol with 40%～80% variable concentrations carries out eluting to macroporous adsorbent resin, follows the tracks of with thin layer chromatography and detects, and collects each stepwise elution liquid of Radix Astragali saponin;
(6) each stepwise elution liquid of Radix Astragali saponin is concentrated, reclaim ethanol, get the Radix Astragali saponin semi-finished product, its content is more than 30%.
(7) with silica gel column chromatography on gained Radix Astragali saponin semi-finished product, and take the volume ratio of methanol and concentrated solution as 1～7: 1 ratio is carried out eluting, and thin layer chromatography is followed the tracks of and detected, and collects each stepwise elution liquid of Radix Astragali saponin;
(8) with collected Radix Astragali saponin eluent, adopt activated carbon decolorizing, recrystallization method to make with extra care to get Radix Astragali saponin, its content is more than 95%.
2. the method for utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali according to claim 1, is characterized in that: in described step (1), cross 40～80 mesh sieves after the Radix Astragali is pulverized.
3. the method for utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali according to claim 2, it is characterized in that: in described step (1), the volume that adds purified water is 10～20 times of Radix Astragali volume.
4. the method for utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali according to claim 3, it is characterized in that: in described step (3), the ultrafiltration molecular cut off is 3000～30000.
5. the method for utilizing Radix Astragali saponin in water vapour reflux, extract, and membrane separation technique and the macroporous adsorbent resin coupled method enriching and purifying Radix Astragali according to claim 4, it is characterized in that: in described step (4), macroreticular resin is a kind of in X-5, NKA-9, S-8, D3520, D4006, H103, D4020, AB-8H and NKA-II type resin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530170A (en) * | 2014-12-08 | 2015-04-22 | 董爱文 | Method for extracting astragaloside IV and astragaloside V from radix astragali |
| CN106107340A (en) * | 2016-06-23 | 2016-11-16 | 甘肃赫博陇药科技有限责任公司 | A kind of antioxidation resisting fatigue Radix Astragali drinks and preparation technology thereof |
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
-
2012
- 2012-12-13 CN CN 201210595622 patent/CN103110689A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530170A (en) * | 2014-12-08 | 2015-04-22 | 董爱文 | Method for extracting astragaloside IV and astragaloside V from radix astragali |
| CN106107340A (en) * | 2016-06-23 | 2016-11-16 | 甘肃赫博陇药科技有限责任公司 | A kind of antioxidation resisting fatigue Radix Astragali drinks and preparation technology thereof |
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
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Address after: 165000 Heilongjiang Province, Jiagedaqi Xinyuan District Changhong community road Beilin Gebe AGA group Applicant after: Daxing'an Mountainrange Lin Gebei psychrophile Science and Technology Co., Ltd. Address before: 165000 Heilongjiang Province, Jiagedaqi Xinyuan District Changhong community road Beilin Gebe AGA group Applicant before: Great Xingan Mountains Lingebei Organic Food Co., Ltd. |
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Application publication date: 20130522 |