CN102391276A - Method for extracting high-purity adenostemmoic acid B from zanthoxylum acanthopodium - Google Patents
Method for extracting high-purity adenostemmoic acid B from zanthoxylum acanthopodium Download PDFInfo
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Abstract
The invention relates to a method for extracting high-purity adenostemmoic acid B from zanthoxylum acanthopodium. The method comprises the following three steps of: 1) ethanol extraction: crushing zanthoxylum acanthopodium rhizomes, adding 0.5 to 5 percent surfactant, performing reflux extraction by adopting ethanol, and concentrating the extract till ethanol smell does not exist; 2) macroporous resin adsorption: separating the obtained concentrate through macroporous adsorption resin, performing gradient elution by using water or ethanol, reclaiming ethanol from the eluent under reduced pressure, and obtaining an extract; and 3) high-speed countercurrent chromatography purification: further purifying the obtained extract by using high-speed countercurrent chromatography, and thus obtaining the adenostemmoic acid B with the purity of over 95 percent. Compared with the conventional extraction process, the method has the advantages that: after the surfactant is added, the extraction rate can be improved, the extraction frequency is reduced, a clear solution can be obtained, and an adsorption column is not blocked during filling; and the method has the advantages of simplicity, convenience, fastness, high preparation quantity, high product purity and the like, and is easy in popularization and use.
Description
Technical field
The invention belongs to natural medicine field, be specifically related to extract in a kind of cluster needling Chinese prickly ash the method for high purity pluviatiol-.
Background technology
Pluviatiol-(Adenostemmoic acid B), molecular formula is C
25H
28O
6, molecular weight is 424.49, is a kind of Lignanoids compounds, is the white granular crystallization, mp.102 ℃ (methyl alcohol).Pharmacological research shows that pluviatiol-has the nervus centralis restraining effect.
The thorn Chinese prickly ash, another name: Zanthoxylum simulans, rock green pepper, derive from Rutaceae thorn Chinese prickly ash (
Zanthoxylum acanthopodiumDC.), be used as medicine with root, fruit.Mainly be distributed in Yunnan, nature and flavor are hot, numb, temperature.Function cures mainly: warming spleen and stomach for dispelling cold, pain relieving, desinsection, contraception; Cure mainly stomachache, rheumatic arthritis, contraception, abdominal pain due to worm stagnation.But thorn Chinese prickly ash chemical constitution study is less, does not also retrieve the technology report that extracts preparation high purity pluviatiol-in the cluster needling Chinese prickly ash in the existing document.
Summary of the invention
The object of the invention just provides the method for extracting the high purity pluviatiol-in a kind of cluster needling Chinese prickly ash, to fill up the blank that present high purity pluviatiol-extracts technology of preparing.
The objective of the invention is to realize through following technical scheme:
1) extraction using alcohol: will sting the Chinese prickly ash rhizome and pulverize, and drop into extractor, and add the ethanol of the 60%-95% that contains 0.5 ~ 5% tensio-active agent, adopt refluxing extraction 2-4 hour, the collection extracting solution is concentrated into does not have the alcohol flavor;
2) macroporous resin adsorption: the gained liquid concentrator is passed through macroporous adsorptive resins; It is colourless earlier to be eluted to effluent with deionized water, water alcohol gradient elution again, and gradient is followed successively by 10%-20% ethanol, 55%-80% ethanol; Collect the elutriant decompression recycling ethanol, obtain extract;
3) high speed adverse current chromatogram purifying: be further purified with high-speed countercurrent chromatography extract obtained, adopting normal hexane-ETHYLE ACETATE-methanol-water is solvent systems, obtains the pluviatiol-of purity more than 95%.
Tensio-active agent hydrophile-lipophile balance value (HLB) is between 14.0 ~ 18.0 in the step 1).
Step 2) the optional AB-8 of said macroporous adsorbent resin, D101, HPD100 isopolarity or nonpolar macroporous adsorption resin.
The said elution system normal hexane-ETHYLE ACETATE of step 3)-methanol-water, its volume ratio is (12-17): (15-25): (8-15): (7-15).
The invention has the beneficial effects as follows:
The present invention adds and shows promoting agent participation extraction, can increase extraction yield, reduces extraction time; Industrial operation can be adopted once or maximum extracted twice, is carrier with low-cost macroporous adsorbent resin, is solvent gradient elution with ethanol; Again through the further separation and purification of high speed adverse current chromatogram; Obtain purity greater than 95% pluviatiol-product, the inventive method operation is simple, fast, environmental protection, product purity is high.
Embodiment
Embodiment 1:
To sting the Chinese prickly ash rhizome and pulverize, and get 5kg and add 30L80% ethanolic soln (containing 0.5%Tween 20) heating and refluxing extraction 2 times, each 4 hours; Filter, merge extracted twice liquid, being evaporated to does not have the alcohol flavor; Through the good D101 macroporous adsorptive resins of pre-treatment, it is colourless to be eluted to elutriant with deionized water earlier, uses 20% ethanol, 55% ethanol elution more successively with liquid concentrator; Collect 55% ethanol eluate, concentrating under reduced pressure obtains stinging the Chinese prickly ash extract.To sting the Chinese prickly ash extract adopts high-speed countercurrent chromatography to carry out purifying; With normal hexane-ETHYLE ACETATE-methanol-water (12:18:8:15) is solvent systems, is moving phase mutually down, on be stationary phase mutually; Collect the pluviatiol-flow point; Reclaim solvent and obtain pluviatiol-, measure through the HPLC method, its purity is 95.4%.
Embodiment 2:
To sting the Chinese prickly ash rhizome and pulverize, and get 5kg and add 50L65% ethanolic soln (containing 1%Tween 80) heating and refluxing extraction 2 times, each 3 hours; Merge extracted twice liquid, being evaporated to does not have the alcohol flavor, with liquid concentrator through the good AB-8 macroporous adsorptive resins of pre-treatment; It is colourless earlier to be eluted to elutriant with deionized water; Use 10% ethanol, 80% ethanol elution more successively, collect 80% ethanol eluate, concentrating under reduced pressure obtains stinging the Chinese prickly ash extract.To sting the Chinese prickly ash extract adopts high-speed countercurrent chromatography to carry out purifying; With normal hexane-ETHYLE ACETATE-methanol-water (15:20:15:7) is solvent systems, is moving phase mutually down, on be stationary phase mutually; Collect the pluviatiol-flow point; Reclaim solvent and obtain pluviatiol-, measure through the HPLC method, its purity is 94.6%.
Embodiment 3:
To sting the Chinese prickly ash rhizome and pulverize, and get 10kg and add 80L72% ethanolic soln (containing 2%Tween 80) heating and refluxing extraction 2 times, extract 3 hours at every turn; Collect extracting solution, being evaporated to does not have the alcohol flavor, with liquid concentrator through the good HPD100 macroporous adsorptive resins of pre-treatment; It is colourless earlier to be eluted to elutriant with deionized water; Use 15% ethanol, 75% ethanol elution more successively, collect 75% ethanol eluate, concentrating under reduced pressure obtains stinging the Chinese prickly ash extract.To sting the Chinese prickly ash extract adopts high-speed countercurrent chromatography to carry out purifying; With normal hexane-ETHYLE ACETATE-methanol-water (14:23:12:10) is solvent systems, is moving phase mutually down, on be stationary phase mutually; Collect the pluviatiol-flow point; Reclaim solvent and obtain pluviatiol-, measure through the HPLC method, its purity is 96.8%.
Embodiment 4:
To sting the Chinese prickly ash rhizome and pulverize, and get 20kg and added 100L95% ethanolic soln (containing 3%Tween 20) heating and refluxing extraction 4 hours, filter; Filter residue added 8L95% ethanolic soln refluxing extraction 2 hours again, filtered, and merged extracted twice liquid; Being evaporated to does not have the alcohol flavor, and through the good AB-8 macroporous adsorptive resins of pre-treatment, it is colourless to be eluted to elutriant with deionized water earlier with liquid concentrator; Use 20% ethanol, 80% ethanol elution more successively, collect 80% ethanol eluate, concentrating under reduced pressure obtains stinging the Chinese prickly ash extract.To sting the Chinese prickly ash extract adopts high-speed countercurrent chromatography to carry out purifying; With normal hexane-ETHYLE ACETATE-methanol-water (17:25:13:9) is solvent systems, is moving phase mutually down, on be stationary phase mutually; Collect the pluviatiol-flow point; Reclaim solvent and obtain pluviatiol-, measure through the HPLC method, its purity is 95.2%.
Embodiment 5:
To sting the Chinese prickly ash rhizome and pulverize, and get 50kg and add 300L60% ethanolic soln (containing 0.8%Tween 20) Suo Shi extraction 4 hours, collect extracting solution; Be evaporated to and do not have the alcohol flavor; Through the good D101 macroporous adsorptive resins of pre-treatment, it is colourless to be eluted to elutriant with deionized water earlier, uses 15% ethanol, 75% ethanol elution more successively with liquid concentrator; Collect 75% ethanol eluate, concentrating under reduced pressure obtains stinging the Chinese prickly ash extract.To sting the Chinese prickly ash extract adopts high-speed countercurrent chromatography to carry out purifying; With normal hexane-ETHYLE ACETATE-methanol-water (13:15:10:15) is solvent systems, is moving phase mutually down, on be stationary phase mutually; Collect the pluviatiol-flow point; Reclaim solvent and obtain pluviatiol-, measure through the HPLC method, its purity is 96.1%.
Claims (4)
1. extract the method for high purity pluviatiol-in the cluster needling Chinese prickly ash, it is characterized in that may further comprise the steps:
1) extraction using alcohol: will sting the Chinese prickly ash rhizome and pulverize, and drop into extractor, and add the ethanol of the 60%-95% that contains 0.5 ~ 5% tensio-active agent, adopt refluxing extraction 2-4 hour, the collection extracting solution is concentrated into does not have the alcohol flavor;
2) macroporous resin adsorption: the gained liquid concentrator is passed through macroporous adsorptive resins; It is colourless earlier to be eluted to effluent with deionized water, water alcohol gradient elution again, and gradient is followed successively by 10%-20% ethanol, 55%-80% ethanol; Collect the elutriant decompression recycling ethanol, obtain extract;
3) high speed adverse current chromatogram purifying: be further purified with high-speed countercurrent chromatography extract obtained, adopting normal hexane-ETHYLE ACETATE-methanol-water is solvent systems, obtains the pluviatiol-of purity more than 95%.
2. the method for extraction high purity pluviatiol-according to claim 1 is characterized in that tensio-active agent hydrophile-lipophile balance value (HLB) is between 14.0 ~ 18.0 in the step 1).
3. the method for extraction high purity pluviatiol-according to claim 1 is characterized in that step 2) the optional AB-8 of said macroporous adsorbent resin, D101, HPD100 isopolarity or nonpolar macroporous adsorption resin.
4. the method for extraction high purity pluviatiol-according to claim 1 is characterized in that the said elution system normal hexane-ETHYLE ACETATE of step 3)-methanol-water, and its volume ratio is (12-17): (15-25): (8-15): (7-15).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905018A (en) * | 2020-09-21 | 2020-11-10 | 中国科学院西双版纳热带植物园 | Preparation method and application of zanthoxylum bungeanum maxim extract |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905018A (en) * | 2020-09-21 | 2020-11-10 | 中国科学院西双版纳热带植物园 | Preparation method and application of zanthoxylum bungeanum maxim extract |
| CN111905018B (en) * | 2020-09-21 | 2022-04-01 | 中国科学院西双版纳热带植物园 | Preparation method and application of zanthoxylum bungeanum maxim extract |
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Application publication date: 20120328 |