CN101596226A - A kind of preparation method of Herba Epimedii total flavones - Google Patents
A kind of preparation method of Herba Epimedii total flavones Download PDFInfo
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- CN101596226A CN101596226A CNA2008101500413A CN200810150041A CN101596226A CN 101596226 A CN101596226 A CN 101596226A CN A2008101500413 A CNA2008101500413 A CN A2008101500413A CN 200810150041 A CN200810150041 A CN 200810150041A CN 101596226 A CN101596226 A CN 101596226A
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- herba epimedii
- total flavones
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- epimedii total
- decolouring
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Abstract
A kind of preparation method of Herba Epimedii total flavones, relate to Chinese crude drug effective site extraction process technology field, the preparation method of Herba Epimedii total flavones specifically proposes the preparation method of a kind of technological process weak point, total flavones yield height, Herba Epimedii total flavones that purity is high.This method is raw material with the Herba Epimedii, Herba Epimedii is added boil extraction in the entry, and filtrate directly feeds LSA class macroporous resin adsorption, eluting, decolouring, reclaim the ethanol drying handle the Herba Epimedii total flavones goods.Technological process of the present invention is short, pollution-free, utilization rate of equipment and installations is high, Herba Epimedii total flavones yield height, and the purity height, production cost is low, and Herba Epimedii total flavones extraction rate reached 4-6% extracts the rate of transform and reaches more than 90%.
Description
Technical field
The present invention relates to Chinese crude drug effective site extraction process technology field, specifically the preparation method of Herba Epimedii total flavones.
Background content
Herba Epimedii is the aerial parts of Berberidaceae Berberridaceae Epimedium Epimedium platymiscium, and there is more than 20 kind in the whole nation, and it is over half to account for global resources, and only Chinese Pharmacopoeia records 5 kinds, its effect: kidney-replenishing, bone and muscle strengthening, wind-damp dispelling.Be used for the seminal emission of sun committee, the muscles and bones flaccidity is soft, and rheumatic arthralgia is numb inflexible twin, climacteric hypertension etc.Its Main Ingredients and Appearance is a Herba Epimedii total flavones, is widely used in medicine and healthy food industry.The extraction process of Herba Epimedii total flavones, traditional method are that water decocts (or alcohol extraction), and ethyl acetate (or n-butyl alcohol) extract repeatedly again, and owing to the organic solvent large usage quantity, method is more numerous and diverse, and extraction cost height, purity are low.For reducing cost, improve purity, so study new extracting method.As the patent No. is " 200310116004.8 ", denomination of invention is " a Herba Epimedii total flavones novel technology for extracting ", disclose a kind of Herba Epimedii total flavones new technology, this invention is to extract solvent with water, adopt the method for resin column purification can make the purity of product bring up to 70%, the yield of total flavones is about 3%.Its weak point is that technological process is long, cost is high, yield is low.
Summary of the invention
The technical problem to be solved in the present invention is: the preparation method that proposes a kind of technological process weak point, total flavones yield height, Herba Epimedii total flavones that purity is high.
The technical scheme of technical solution problem of the present invention is: be raw material with the Herba Epimedii, Herba Epimedii added boil extraction in the entry, filter, filtrate directly feeds LSA class macroporous resin adsorption, water flushing resin column is closely colourless to effluent, use 5-8 instead and doubly measure the 20-95% ethanol gradient elution, decolouring, reclaim the ethanol drying handle the Herba Epimedii total flavones goods.
The described decolouring of the technical scheme of technical solution problem of the present invention is that eluent is fed the resin column decolouring.
The decolour resin model of usefulness of the present invention is the LSI resinoid.
The invention has the beneficial effects as follows: the present invention's water extraction Herba Epimedii total flavones, with the special-purpose Herba Epimedii total flavones adsorbent resin of LSA class, as homemade LSA-5B resin (adsorbing material responsibility company limited is changed in the blue deep friendship in Xi'an to be provided), make Herba Epimedii total flavones extraction rate reached 4-6%, extracting the rate of transform reaches more than 90%, purity (UVI method mensuration) content reaches more than 95%, and (HPLC method mensuration) content reaches more than 60%.The technological process of employing LSA resinoid extraction Herba Epimedii total flavones is short, pollution-free, utilization rate of equipment and installations is high, Herba Epimedii total flavones yield height, and the purity height, production cost is low.
The specific embodiment
The present invention is further described in conjunction with embodiment as described below:
Embodiment 1
With the 100kg Herba Epimedii is raw material, Herba Epimedii added to boil in the entry carry 3 times, each amount of water is respectively 10 of Herba Epimedii weight, 8,8 times, extraction time was respectively 2 hours, 1.5 and 1.5 hours, merge extractive liquid,, filter, filtrate is fed the LSA-5B macroporous resin adsorption, after treating that the effluent detection is saturated, water flushing pillar is closely colourless to effluent, then with 2 times of amount 20% ethanol elutions, the ethanol elution of 3 times of amounts 70% of reuse, with 2 times of amount 95% ethanol elutions, merge and collect eluent then, feed the decolouring of LSI-632 resin column, destaining solution reclaims ethanol to relative density 1.15-1.20, to remove alcoholic acid fluid extract in dry below 80 ℃, and get Herba Epimedii total flavones 4.97kg, content is 95.6%.
Embodiment 2
With the 100kg Herba Epimedii is raw material, Herba Epimedii added to boil in the entry carry 3 times, each amount of water is respectively 10 of Herba Epimedii weight, 8,8 times, extraction time was respectively 2 hours, 1.5 and 1.5 hours, merge extractive liquid,, filter, filtrate is fed the LSA-20 macroporous resin adsorption, after treating that the effluent detection is saturated, water flushing pillar is closely colourless to effluent, earlier with 2 times of amount 20% ethanol elutions, the ethanol elution of 4 times of amounts 60% of reuse, with 2 times of amount 95% ethanol elutions, right collection eluent feeds the decolouring of LSI-632 resin column then, collect destaining solution and reclaim ethanol to relative density 1.15-1.20, to remove alcoholic acid fluid extract in 80 ℃ of dryings, and get Herba Epimedii total flavones 5.03kg, content is 94.2%.
Embodiment 3
With the 100kg Herba Epimedii is raw material, Herba Epimedii added to boil in the entry carry 3 times, each amount of water is respectively 10 of Herba Epimedii weight, 8,8 times, extraction time was respectively 2 hours, 1.5 and 1.5 hours, merge extractive liquid,, filter, filtrate is fed the LSA-10 macroporous resin adsorption, after treating that the effluent detection is saturated, water flushing pillar is closely colourless to effluent, then with 2 times of amount 20% ethanol elutions, the ethanol elution of 3 times of amounts 70% of reuse, with 2 times of amount 95% ethanol elutions, merge and collect eluent at last, feed the decolouring of LSI-632 post, collect destaining solution and reclaim ethanol to relative density 1.15-1.20, to remove alcoholic acid fluid extract in 80 ℃ of dryings, and get Herba Epimedii total flavones 4.87kg, content is 93.8%.
Embodiment 4
With the 100kg Herba Epimedii is raw material, Herba Epimedii added to boil in the entry carry 3 times, each amount of water is respectively 10 of Herba Epimedii weight, 8,8 times, extraction time was respectively 2 hours, 1.5 and 1.5 hours, merge extractive liquid,, filter, filtrate is fed the LSA-7 macroporous resin adsorption, after treating that the effluent detection is saturated, water flushing pillar is closely colourless to effluent, earlier with 2 times of amount 20% ethanol elutions, the ethanol elution of 3 times of amounts 75% of reuse, with 2 times of amount 95% ethanol elutions, merge and collect eluent at last, feed the decolouring of LST-632 post, collect destaining solution and reclaim ethanol to relative density 1.15-1.20, to remove alcoholic acid fluid extract in 80 ℃ of dryings, and get Herba Epimedii total flavones 4.63kg, content is 91.2%.
Claims (3)
- The preparation method of 1 one kinds of Herba Epimedii total flavones, it is characterized in that: be raw material with the Herba Epimedii, Herba Epimedii added boil extraction in the entry, filter, filtrate directly feeds LSA class macroporous resin adsorption, and water flushing resin column is closely colourless to effluent, uses 5-8 instead and doubly measures the 20-95% ethanol gradient elution, decolouring, reclaim the ethanol drying handle the Herba Epimedii total flavones goods.
- 2 according to the said preparation method of claim 1, it is characterized in that: said decolouring is that eluent is fed the resin column decolouring.
- 3 according to the said preparation method of claim 2, it is characterized in that: the resin model of decolouring usefulness is the LSI resinoid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101500413A CN101596226A (en) | 2008-06-04 | 2008-06-04 | A kind of preparation method of Herba Epimedii total flavones |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101500413A CN101596226A (en) | 2008-06-04 | 2008-06-04 | A kind of preparation method of Herba Epimedii total flavones |
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| CN101596226A true CN101596226A (en) | 2009-12-09 |
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| CNA2008101500413A Pending CN101596226A (en) | 2008-06-04 | 2008-06-04 | A kind of preparation method of Herba Epimedii total flavones |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466385A (en) * | 2021-08-13 | 2021-10-01 | 五源本草(山东)健康科技有限公司 | Selaginella pulvinata total flavone extraction preparation and HPLC fingerprint detection method |
| WO2023060622A1 (en) * | 2021-10-17 | 2023-04-20 | 南通市台盈新材料科技有限公司 | Enrichment tube for enriching total flavones in epimedium brevicomu maxim leaf extracting solution |
-
2008
- 2008-06-04 CN CNA2008101500413A patent/CN101596226A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466385A (en) * | 2021-08-13 | 2021-10-01 | 五源本草(山东)健康科技有限公司 | Selaginella pulvinata total flavone extraction preparation and HPLC fingerprint detection method |
| WO2023060622A1 (en) * | 2021-10-17 | 2023-04-20 | 南通市台盈新材料科技有限公司 | Enrichment tube for enriching total flavones in epimedium brevicomu maxim leaf extracting solution |
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Addressee: Wang Yuanqing Document name: Notification of before Expiration of Request of Examination as to Substance |
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Application publication date: 20091209 |