CN1740184A - A kind of technology of from the Gentiana medicinal plant, extracting the secoiridoid glycosides product - Google Patents
A kind of technology of from the Gentiana medicinal plant, extracting the secoiridoid glycosides product Download PDFInfo
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- CN1740184A CN1740184A CN 200410083087 CN200410083087A CN1740184A CN 1740184 A CN1740184 A CN 1740184A CN 200410083087 CN200410083087 CN 200410083087 CN 200410083087 A CN200410083087 A CN 200410083087A CN 1740184 A CN1740184 A CN 1740184A
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Abstract
The present invention relates to a kind of technology of from the Gentiana medicinal plant, extracting secoiridoid glycoside (bitter glycosides) class product, it is a raw material with Gentiana medicinal plant herb or root, stem, leaf, flower, with the hydrophilic solvent refluxing extraction, and utilization separates and enrichment the macroporous resin that water soluble component has the selective adsorption effect, obtain the secoiridoid glycosides product, wherein the content of secoiridoid glycosides compound is greater than 20%.Technology of the present invention is easy, easy to operate, safety, good reproducibility, but suitability for industrialized production.
Description
Technical field
The present invention relates to the extraction process of Chinese herbal medicine effective ingredients, relate in particular to a kind of technology of from the Gentiana medicinal plant, extracting secoiridoid glycoside (bitter glycosides) class product.
Background technology
Main medicinal plant has bark of ash, radix gentiane dahuvicae, fried dough twist Macrophylla, gentiana crassicaulis Duthie etc. in the agueweed.Qinghai-Tibet rough gentian, Herba Gentianae Urnulae, alpine gentian etc. are many with root, flower or all herbal medicine, have wind-damp dispelling, clearing away damp-heat, stopping numbness pain, multiple efficacies such as clearing heat and detoxicating.Be used for the contraction of muscle arteries and veins clinically, joint is ached, the infantile malnutrition heating, the treatment of various disease conditions such as jaundice [see one one of Pharmacopoeia of People's Republic of China, 2000 editions, the 222-223 page or leaf; Drug Standard of Ministry of Public Health of the Peoples Republic of China, one of Tibetan medicine, 1992; 17 pages, 52 pages].Its medicinal part all contains a large amount of secoiridoid glycoside (bitter glycosides) constituents, not only claims Swertiamain (swertiamarin), sweroside to claim sweroside (sweroside), bitter rough gentian ester glucoside not only but also claim amarogentin (amarogentin) etc. as gentiopicrin (gentiopicroside), when the bitter glycosides of medicine
][＜Acta Pharmaceutica Sinica 〉, 1991; 26 (11) 864-870 pages or leaves: " five kinds of secoiridoid glycosides bitter-taste components high performance liquid chromatography quantitative analysis in nine kinds of rough gentian " (Zhang Jiansheng, by son work such as new);＜high protistology collected papers〉[C], 1992:113-118 page or leaf, " Qinghai-Tibet Platean four kinds of gentianaceae plant chemical ingredients preliminary study [A] " (Ji Lanju, work such as Sun Hongfa);＜pharmaceutical analysis magazine〉1994; 14 (1) 41-43 pages or leaves " the RP-HPLC method of gentiopicroside is measured in the bark of ash " (Sun Wenji, the sand side of shaking etc.).In these secoiridoid glycosides (bitter glycosides) constituents, gentiopicrin has the gastric juice of promotion and the free hydrochloric acid excretory is good for the stomach and anti-inflammatory action, when the bitter glycosides of medicine has the hair growth of promotion and spasmolysis, analgesic and anti-inflammatory effects, sweroside has the anticonvulsant action of bringing down a fever and anti-hepatocellular injury, and the hepatoprotective effect that the promotion liver cell is repaired [＜bulletin of Chinese materia medica〉1986; 11 (11) 643-647: " Chinese Gentianaceae medicinal plant overview " (Song Wanzhi);＜middle pharmaceutically active ingredient pharmacology and application〉1994; 454-455 (Ji Yubin etc.)].With this constituents is the main anodyne of developing, and Antihepatitis medicament has suitability for industrialized production, but the Study on extraction of relevant this constituents report is still few.Bibliographical information, the content of gentiopicroside is very high in bark of ash and the fried dough twist Macrophylla root, generally between 3～13% (w/w) [＜northwest Botany Gazette〉2004; 24 (2) 292-2958, " assay of iridoids composition and quality evaluation in the Tibetan medicine gentiana straminea maxim " (Ji Lanju, Ma Yuhua etc.)], along with the cultivation success of medicinal bark of ash, fried dough twist Macrophylla, formed abundant, the medicine resource that the utmost point has exploitation to be worth.
The extraction separation of the water soluble component of natural product, macroreticular resin absorbing method is a kind of very effective industrialized preparing process, utilize polymeric adsorbent from the Gentiana medicinal plant, to extract the industrialized preparing process of secoiridoid glycoside (bitter glycosides) class, have not yet to see both at home and abroad about document and patent report.
Summary of the invention
The purpose of this invention is to provide a kind of technology of from the Gentiana medicinal plant, extracting secoiridoid glycoside (bitter glycosides) compounds.
Purpose of the present invention can realize by following measure:
A kind of technology of from Gentiana section medicinal plant, extracting the secoiridoid glycosides product, may further comprise the steps: 1. with dry Gentiana medicinal plant powder with hydrophilic organic solvent 50-80 ℃ of following refluxing extraction 2-4 time, each 2-4 hour, the filtered and recycled organic solvent got secoiridoid glycosides extracting solution and united extraction liquid; 2. enrichment step 1. the gained extracting solution to do the secoiridoid glycosides product; Or make step 1. the gained extracting solution slowly flow through with ethanol swelling and the macroporous adsorption resin chromatography post crossed through water elution, use aqueous ethanolic solution or the above-mentioned resin chromatography column of the slow wash-out of 0-50% methanol aqueous solution of 0-50% again, collect elutriant and be concentrated into dried light brown secoiridoid glycosides product.
1. add an amount of water in the gained extracting solution in above-mentioned steps, and room temperature or 0～4 ℃ refrigeration 12～48 hours muddy liquid, centrifugal or filter and obtain clear liquor, clear liquor is slowly flow through with ethanol swelling and the macroporous adsorption resin chromatography post crossed through water elution.
After 2. above-mentioned steps is finished, earlier slowly clean the resin chromatography column with an amount of water, and then with the above-mentioned macroporous adsorption resin chromatography post of the slow wash-out of methanol aqueous solution of 0～50% aqueous ethanolic solution or 0～50% and collect elutriant.
Described hydrophilic organic solvent is methanol solution or ethanolic soln or methanol aqueous solution or aqueous ethanolic solution or the methyl alcohol and the alcoholic acid aqueous solution.
Advantage of the present invention:
1, the present invention is a raw material with Gentiana medicinal plant herb or root, stem, leaf, flower, with the hydrophilic solvent refluxing extraction, and utilization separates and enrichment the macroporous resin that water soluble component has the selective adsorption effect, obtain the secoiridoid glycosides product, the content of secoiridoid glycosides compound is greater than 20% in this extract.
2, easy, easy to operate, the safety of technology of the present invention, good reproducibility, but suitability for industrialized production.
Embodiment
Embodiment one: a kind of technology of extracting the secoiridoid glycosides product from Gentiana medicinal plant fried dough twist Macrophylla plant, may further comprise the steps: earlier with the dry root of fried dough twist Macrophylla plant with the methanol aqueous solution of 20-95% the 50-80 ℃ of consumption refluxing extraction three times of successively decreasing successively, each 2-4 hour, filter and reclaim the extracting solution that methanol solution gets the secoiridoid glycosides product, and merge the extracting solution that concentrates three backflows; Add an amount of water in the extracting solution after appropriateness concentrates and get muddy liquid, and left standstill under the room temperature 24-48 hour putting, filter or centrifugal removal flocculation fat-soluble component gets clear liquor and is concentrated into dried driffractive ring alkene terpene glycoside product, the content of secoiridoid glycosides compound is greater than 15% in this product.
Embodiment two: a kind ofly belong to the medicinal plant fried dough twist Macrophylla plant technology of extracting the secoiridoid glycosides product from Gentianaceae, may further comprise the steps: (1) with the dry stem of fried dough twist Macrophylla plant with methanol solution the 50-80 ℃ of consumption refluxing extraction three times of successively decreasing successively, each 2-4 hour, filter and reclaim the extracting solution that methanol solution gets the secoiridoid glycosides product, and merge the extracting solution that concentrates three backflows; (2) add an amount of water in the extracting solution after appropriateness concentrates and get muddy liquid, and left standstill 24-48 hour 0～4 ℃ of refrigeration, filtration or centrifugal removal flocculation fat-soluble component get clear liquor; (3), with adequate amount of ethanol swelling and, make it to carry out the transition to gradually water, and to change it over to internal diameter be that internal diameter is that 1-30cm, footpath degree are 1: formation resin chromatography column in the chromatography column of 2-20 through water elution with a certain amount of macroporous adsorbent resin; (4) step (2) gained clear liquor is slowly flow through above-mentioned resin chromatography column with the flow velocity of 1BV/h; (5) slowly clean above-mentioned resin chromatography column with suitable quantity of water earlier, and then with the ethanolic soln of 0-50% with the flow velocity of 0.5BV/h slow wash-out resin chromatography column and collect elutriant, be concentrated into driedly, obtain brown extract, the content of secoiridoid glycosides compound is greater than 20% in this extract.
Embodiment three: a kind ofly belong to the medicinal plant fried dough twist Macrophylla plant technology of extracting the secoiridoid glycosides product from Gentianaceae, may further comprise the steps: (1) with the dry stem of fried dough twist Macrophylla plant with methanol solution the 50-80 ℃ of consumption refluxing extraction three times of successively decreasing successively, each 2-4 hour, filter and reclaim the extracting solution that methanol solution gets the secoiridoid glycosides product, and merge the extracting solution that concentrates three backflows; (2) add an amount of water in the extracting solution after appropriateness concentrates and get muddy liquid, and at room temperature left standstill 24-48 hour, filtration or centrifugal removal flocculation fat-soluble component get clear liquor; (3), with adequate amount of ethanol swelling and, make it to carry out the transition to gradually water, and to change it over to internal diameter be that internal diameter is that 1-30cm, footpath degree are 1: formation resin chromatography column in the chromatography column of 2-20 through water elution with a certain amount of macroporous adsorbent resin; (4) step (2) gained clear liquor is slowly flow through above-mentioned resin chromatography column with the flow velocity of 1BV/h; (5) slowly clean above-mentioned resin chromatography column with suitable quantity of water earlier, and then with the methanol solution of 0-50% with the flow velocity of 0.5BV/h slow wash-out resin chromatography column and collect elutriant, be concentrated into driedly, obtain brown extract, the content of secoiridoid glycosides compound is greater than 20% in this extract.
Embodiment four: a kind of technology of extracting the secoiridoid glycosides product from Gentiana medicinal plant fried dough twist Macrophylla plant, may further comprise the steps: with the dry herb of fried dough twist Macrophylla plant with ethanolic soln the 50-80 ℃ of consumption refluxing extraction three times of successively decreasing successively, each 2-4 hour, filter and reclaim the extracting solution that methanol solution gets the secoiridoid glycosides product, and merge the extracting solution that concentrates three backflows; In the extracting solution that concentrates appropriateness, add an amount of water and get muddy liquid, and left standstill 24-48 hour 0～4 ℃ of refrigeration, filter or centrifugal removal flocculation fat-soluble component gets clear liquor and is concentrated into dried driffractive ring alkene terpene glycoside product, the content of secoiridoid glycosides compound is greater than 15% in this product.
Embodiment five: a kind of technology of extracting the secoiridoid glycosides product from Gentiana medicinal plant fried dough twist Macrophylla, may further comprise the steps: (1) with the dry herb of fried dough twist Macrophylla plant with 50% aqueous ethanolic solution the 50-80 ℃ of consumption refluxing extraction three times of successively decreasing successively, each 2-4 hour, filter and reclaim the extracting solution that methanol solution gets the secoiridoid glycosides product, and merge the extracting solution that concentrates three backflows; (2) add an amount of water in the extracting solution of above-mentioned concentrated appropriateness and get muddy liquid, and left standstill 24-48 hour 0～4 ℃ of refrigeration, filtration or centrifugal removal flocculation fat-soluble component get clear liquor; (3) with a certain amount of macroporous adsorbent resin, make it to carry out the transition to gradually water with the adequate amount of ethanol swelling and through water elution, and to change it over to internal diameter be that internal diameter is that 1-30cm, footpath degree are 1: in the chromatography column of 2-20, form the resin chromatography column; (4) step (2) gained clear liquor is slowly flow through above-mentioned resin chromatography column with the flow velocity liquid of 1BV/h; (5) slowly clean the resin chromatography column with suitable quantity of water earlier, and then with the ethanolic soln of 0-50% with the flow velocity of 0.5BV/h slow wash-out resin chromatography column and collect elutriant, concentrate eluant obtains brown secoiridoid glycosides extract to dried, and the content of secoiridoid glycosides compound is greater than 20% in this extract.
Embodiment six: a kind of technology of extracting the secoiridoid glycosides product from Gentiana medicinal plant fried dough twist Macrophylla, may further comprise the steps: (1) with the dry herb of fried dough twist Macrophylla plant with 50% aqueous ethanolic solution the 50-80 ℃ of consumption refluxing extraction three times of successively decreasing successively, each 2-4 hour, filter and reclaim the extracting solution that methanol solution gets the secoiridoid glycosides product, and merge the extracting solution that concentrates three backflows; (2) add an amount of water in the extracting solution of above-mentioned concentrated appropriateness and get muddy liquid, and at room temperature left standstill 24-48 hour, filtration or centrifugal removal flocculation fat-soluble component get clear liquor; (3) with a certain amount of macroporous adsorbent resin, make it to carry out the transition to gradually water with the adequate amount of ethanol swelling and through water elution, and to change it over to internal diameter be that internal diameter is that 1-30cm, footpath degree are 1: in the chromatography column of 2-20, form the resin chromatography column; (4) step (2) gained clear liquor is slowly flow through above-mentioned resin chromatography column with the flow velocity liquid of 1BV/h; (5) slowly clean the resin chromatography column with suitable quantity of water earlier, and then with the methanol solution of 0-50% with the flow velocity of 0.5BV/h slow wash-out resin chromatography column and collect elutriant, concentrate eluant obtains brown secoiridoid glycosides extract to dried, and the content of secoiridoid glycosides compound is greater than 20% in this extract.
Other are the same with the technology that Gentiana medicinal plant (as radix gentiane dahuvicae, gentiana crassicaulis Duthie etc.) extracts the secoiridoid glycosides product.
Claims (4)
1, a kind of technology of from Gentiana section medicinal plant, extracting the secoiridoid glycosides product, may further comprise the steps: 1. with dry Gentiana medicinal plant with hydrophilic organic solvent 50-80 ℃ of following refluxing extraction 2-4 time, each 2-4 hour, the filtered and recycled organic solvent got secoiridoid glycosides extracting solution and united extraction liquid; 2. enrichment step 1. the gained extracting solution to do the secoiridoid glycosides product; Or make step 1. the gained extracting solution slowly flow through with ethanol swelling and the macroporous adsorption resin chromatography post crossed through water elution, use aqueous ethanolic solution or the above-mentioned resin chromatography column of the slow wash-out of 0-50% methanol aqueous solution of 0-50% again, collect elutriant and be concentrated into dried light brown secoiridoid glycosides product.
2, the technology of from the Gentiana medicinal plant, extracting the secoiridoid glycosides product as claimed in claim 1, it is characterized in that: 1. add an amount of water in the gained extracting solution to step, and room temperature or 0～4 ℃ refrigeration 12～48 hours muddy liquid, centrifugal or filter and to obtain clear liquor, clear liquor is slowly flow through with ethanol swelling and the macroporous adsorption resin chromatography post crossed through water elution.
3, the technology of from the Gentiana medicinal plant, extracting the secoiridoid glycosides product as claimed in claim 1 or 2, it is characterized in that: after 2. step is finished, earlier slowly clean the resin chromatography column with an amount of water, and then with the above-mentioned macroporous adsorption resin chromatography post of the slow wash-out of methanol aqueous solution of 0～50% aqueous ethanolic solution or 0～50% and collect elutriant.
4, the technology of extracting the secoiridoid glycosides product from the Gentiana medicinal plant as claimed in claim 1, it is characterized in that: described hydrophilic organic solvent is methanol solution or ethanolic soln or methanol aqueous solution or aqueous ethanolic solution or the methyl alcohol and the alcoholic acid aqueous solution.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104857008A (en) * | 2015-04-22 | 2015-08-26 | 宁夏医科大学 | Application of Gentiopicroside, Gent as a medicament for the treatment of neuropathic pain |
| CN105878362A (en) * | 2014-09-30 | 2016-08-24 | 复旦大学 | Application of gentian iridoid glycosides in preparation of medicine for treating liver injury |
| CN106137812A (en) * | 2015-04-03 | 2016-11-23 | 伽蓝（集团）股份有限公司 | Radix Gentianae extract and its production and use |
| CN106137811A (en) * | 2015-04-03 | 2016-11-23 | 伽蓝（集团）股份有限公司 | A kind of composition of plant extracts and application thereof |
| CN106674312A (en) * | 2017-01-06 | 2017-05-17 | 成都彼斯特生物科技有限公司 | Separation and purification method for high-purity monomer sweroside series components |
| CN107163095A (en) * | 2017-06-07 | 2017-09-15 | 上海中药标准化研究中心 | Urnu gentian herb glycosides A extracting method and its purposes for preparing cough suppressing medicine |
| CN109172633A (en) * | 2018-10-19 | 2019-01-11 | 中国科学院西北高原生物研究所 | A kind of Radix Gentianae Macrophyllae extract and the preparation method and application thereof |
-
2004
- 2004-08-26 CN CN 200410083087 patent/CN1740184A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105878362A (en) * | 2014-09-30 | 2016-08-24 | 复旦大学 | Application of gentian iridoid glycosides in preparation of medicine for treating liver injury |
| CN106137812A (en) * | 2015-04-03 | 2016-11-23 | 伽蓝（集团）股份有限公司 | Radix Gentianae extract and its production and use |
| CN106137811A (en) * | 2015-04-03 | 2016-11-23 | 伽蓝（集团）股份有限公司 | A kind of composition of plant extracts and application thereof |
| CN104857008A (en) * | 2015-04-22 | 2015-08-26 | 宁夏医科大学 | Application of Gentiopicroside, Gent as a medicament for the treatment of neuropathic pain |
| CN106674312A (en) * | 2017-01-06 | 2017-05-17 | 成都彼斯特生物科技有限公司 | Separation and purification method for high-purity monomer sweroside series components |
| CN107163095A (en) * | 2017-06-07 | 2017-09-15 | 上海中药标准化研究中心 | Urnu gentian herb glycosides A extracting method and its purposes for preparing cough suppressing medicine |
| CN109172633A (en) * | 2018-10-19 | 2019-01-11 | 中国科学院西北高原生物研究所 | A kind of Radix Gentianae Macrophyllae extract and the preparation method and application thereof |
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