CN103664987B - Artemisinin and preparation method thereof - Google Patents
Artemisinin and preparation method thereof Download PDFInfo
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- CN103664987B CN103664987B CN201310725567.0A CN201310725567A CN103664987B CN 103664987 B CN103664987 B CN 103664987B CN 201310725567 A CN201310725567 A CN 201310725567A CN 103664987 B CN103664987 B CN 103664987B
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- artemisinin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/20—Spiro-condensed systems
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Abstract
The invention discloses a kind of preparation method of Artemisinin, it is dry by raw medicinal material sweet wormwood and be crushed to 20-80 order that the method comprises (1); (2) be that solvent carries out refluxing extraction twice to material with ethyl acetate, merge extracted twice liquid and concentrate, for subsequent use, in leaching process, step vacuumizing and vacuum breaker is carried out to extractor; (3) by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then the ethanol of 90-99.7% carries out wash-out, and elutriant, through the ethyl alcohol recrystallization of concentrated, crystallization and 50-90%, namely obtains Artemisinin product after drying.The present invention is by extracting vacuum impulse formula and macroporous resin adsorption combination, and achieve from sweet wormwood, prepare Artemisinin low cost and High-efficient Production, market application foreground is wide.
Description
Technical field
The present invention relates to a kind of preparation method of Artemisinin, specifically refer to the method for extraction purification Artemisinin from Chinese medicinal materials sweet wormwood.
Background technology
Artemisinin is the sesquiterpene lactones new antimalarial agent having peroxy-radical extracted from Chinese medicine sweet wormwood, synthesize multiple derivative on its basis, as dihydroarteannuin, Artemether, Artesunate etc., artemisinin-based drug, because toxicity is low, anti-cruel property is strong, thus has very important pharmaceutical use.
Artemisinin is colourless acicular crystal, bitter, be soluble in acetone, vinyl acetic monomer, chloroform, in benzene and the more weak organic solvent of sherwood oil isopolarity, thus from sweet wormwood, extract Artemisinin generally all adopts these organic solvents as extraction agent, but the main component of sweet wormwood is the strong polarity such as Mierocrystalline cellulose and pectin and hydrophilic material, the penetrance of these solvents to strong polarity and hydroaropic substance is poor, Artemisinin is wrapped up by the plant cell tissue being main component with Mierocrystalline cellulose and pectin again, thus there is very large resistance to mass transfer in these solvents in leaching process, solvent is difficult to go to dissolve Artemisinin through plant cell tissue, the solution having dissolved Artemisinin is also difficult to discharge, extraction time is long and efficiency is low, the residual rate of Artemisinin is often also higher.
On the other hand, because the artemislnin content in sweet wormwood is lower, also bring a large amount of impurity in leaching process thereupon, thus need to carry out purifying, purifying process present stage mainly adopts silica gel column chromatography, but yield is low, cost is high shortcoming that silica gel column chromatography exists, thus, prior art can not meet the requirement that Artemisinin is produced.
Summary of the invention
For solving the above-mentioned prior art Problems existing extracting Artemisinin from sweet wormwood, the present inventor is through a large amount of scientific practices, finally invent that a kind of extraction efficiency is high, Artemisinin residual rate is low, the Artemisinin preparation method that in purge process, product yield is high, cost is low.
The present invention includes following step:
(1) process of raw medicinal material: raw medicinal material sweet wormwood is dry and be crushed to 20-80 order.
(2) extraction of Artemisinin: be that solvent carries out refluxing extraction twice to material with ethyl acetate, during extraction, the volume mass of solvent and material is than being 2:1-12:1, extraction time 1-5 hour, merges extracted twice liquid and concentrates, for subsequent use.In volume mass ratio, the unit of volume is milliliter, and the unit of quality is gram.
In said extracted process, step vacuumizing and vacuum breaker is carried out to extractor, utilize vacuum impulse reinforcing mass transfer.The mechanism of vacuum impulse reinforcing mass transfer is: because ethyl acetate is the weakly polar organic solvent that volatility is stronger, ethyl acetate when vacuumizing in sweet wormwood cell tissue can gasify because of decompression, cause sweet wormwood histocyte internal pressure to be greater than outside sweet wormwood histocyte, the ethyl acetate of having dissolved Artemisinin can be forced through sweet wormwood cell tissue under differential pressure action; When vacuum breaker, sweet wormwood histocyte external pressure is greater than pressure in sweet wormwood histocyte, ethyl acetate outside sweet wormwood histocyte enters rapidly sweet wormwood histocyte inside and goes to dissolve Artemisinin because of differential pressure action, the change that replaces of this sweet wormwood histocyte external and internal pressure enhances solvent and dissolving Artemisinin mass transfer in a solvent, makes extraction efficiency raising, the reduction of Artemisinin residual rate.
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then the ethanol of 90-99.7% carries out wash-out, elutriant is through the ethyl alcohol recrystallization of concentrated, crystallization and 50-90%, namely obtain Artemisinin product after drying, in product, the massfraction of Artemisinin can reach 99.5%-99.99%.
After wash-out completes, ethanol elution for some time of continuation 90-99.7% can realize the activation of macroporous adsorbent resin and reuse, general reusable 3-5 time of resin.
Compared with prior art, the invention has the beneficial effects as follows: step vacuumizing and vacuum breaker is carried out to extractor, adopt vacuum impulse reinforcing mass transfer, effectively shorten extraction time, improve the extraction yield of Artemisinin; Adopt vacuum impulse formula to be extracted in and shorten extraction time and also reduce the requirement to equipment while ensureing extraction yield, common refluxing extraction tank can realize through simple transformation, reduces cost; The purifying of Artemisinin adopts the ethanol elution of semipolar absorption with macroporous adsorbent resin, high density, the use of macroporous resin and activation one step is completed, decreases operation steps, reduces cost.
In sum, the present invention is by extracting vacuum impulse formula and macroporous resin adsorption combination, achieve low cost and the High-efficient Production of extraction and isolation Artemisinin from sweet wormwood, prove through test, this technique is used to carry out extraction and isolation to Artemisinin, product yield can improve 3%-5%, cost reduces 5%-8%, and market application foreground is wide.
Embodiment
Below the preparation method of Artemisinin is described in detail.
Embodiment 1:
(1) process of raw medicinal material: raw medicinal material sweet wormwood is dry and be crushed to 25 orders.
(2) extraction of Artemisinin: be that solvent carries out refluxing extraction twice to material with ethyl acetate, during extraction, solvent and the volume mass of material are than being 3:1,4.5 hours extraction times, merge extracted twice liquid and concentrate, for subsequent use, in volume mass ratio, the unit of volume is milliliter, and the unit of quality is gram, in leaching process, step vacuumizing and vacuum breaker is carried out to extractor, utilize vacuum impulse reinforcing mass transfer.
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then the ethanol of 91% carries out wash-out, elutriant through concentrated, crystallization and 60% ethyl alcohol recrystallization, namely obtain Artemisinin product after drying, in product, the massfraction of Artemisinin is 99.58%.
After wash-out completes, continue namely to realize the activation of macroporous adsorbent resin with ethanol elution for some time of 95%.
Embodiment 2:
(1) process of raw medicinal material: raw medicinal material sweet wormwood is dry and be crushed to 40 orders.
(2) extraction of Artemisinin: be that solvent carries out refluxing extraction twice to material with ethyl acetate, during extraction, solvent and the volume mass of material are than being 6:1,3 hours extraction times, merge extracted twice liquid and concentrate, for subsequent use, in volume mass ratio, the unit of volume is milliliter, and the unit of quality is gram, in leaching process, step vacuumizing and vacuum breaker is carried out to extractor, utilize vacuum impulse reinforcing mass transfer.
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then the ethanol of 95% carries out wash-out, elutriant through concentrated, crystallization and 75% ethyl alcohol recrystallization, namely obtain Artemisinin product after drying, in product, the massfraction of Artemisinin is 99.75%.
After wash-out completes, continue namely to realize the activation of macroporous adsorbent resin with ethanol elution for some time of 92%.
Embodiment 3:
(1) process of raw medicinal material: raw medicinal material sweet wormwood is dry and be crushed to 70 orders.
(2) extraction of Artemisinin: be that solvent carries out refluxing extraction twice to material with ethyl acetate, during extraction, solvent and the volume mass of material are than being 10:1,1.5 hours extraction times, merge extracted twice liquid and concentrate, for subsequent use, in volume mass ratio, the unit of volume is milliliter, and the unit of quality is gram, in leaching process, step vacuumizing and vacuum breaker is carried out to extractor, utilize vacuum impulse reinforcing mass transfer.
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then the ethanol of 99% carries out wash-out, elutriant through concentrated, crystallization and 88% ethyl alcohol recrystallization, namely obtain Artemisinin product after drying, in product, the massfraction of Artemisinin is 99.91%.
After wash-out completes, continue namely to realize the activation of macroporous adsorbent resin with ethanol elution for some time of 98%.
Claims (1)
1. a preparation method for Artemisinin, is characterized in that comprising following step:
(1) process of raw medicinal material: raw medicinal material sweet wormwood is dry and be crushed to 20-80 order;
(2) extraction of Artemisinin: be that solvent carries out refluxing extraction twice to material with ethyl acetate, during extraction, solvent and the volume mass of material are than being 2:1-12:1, extraction time 1-5 hour, merge extracted twice liquid and concentrate, for subsequent use, in leaching process, step vacuumizing and vacuum breaker is carried out to extractor;
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then the ethanol of 90-99.7% carries out wash-out, and the ethanol elution of continuation 90-99.7% after wash-out completes, realizes the activation of macroporous adsorbent resin; Elutriant, through the ethyl alcohol recrystallization of concentrated, crystallization and 50-90%, namely obtains Artemisinin product after drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310725567.0A CN103664987B (en) | 2013-12-25 | 2013-12-25 | Artemisinin and preparation method thereof |
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| CN201310725567.0A CN103664987B (en) | 2013-12-25 | 2013-12-25 | Artemisinin and preparation method thereof |
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| CN103664987A CN103664987A (en) | 2014-03-26 |
| CN103664987B true CN103664987B (en) | 2016-01-20 |
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| CN105924453A (en) * | 2016-06-14 | 2016-09-07 | 南京市建邺区景春堂电子商务中心 | Artemisinin extraction method and artemisinin extract |
| CN108299459B (en) * | 2018-03-16 | 2020-06-19 | 中国科学院过程工程研究所 | Method for extracting artemisinin by using polyethylene glycol solvent |
| CN114271533B (en) * | 2022-02-14 | 2023-01-31 | 云南中烟工业有限责任公司 | Method for improving flue gas quality of sun-cured tobacco |
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| US4952603A (en) * | 1988-06-20 | 1990-08-28 | Elferaly Farouk S | Method for the isolation of artemisinin from Artemisia annua |
| CN1554290A (en) * | 2003-12-22 | 2004-12-15 | 郭以顺 | Leaching process for dry fruit |
| CN101130548B (en) * | 2006-08-25 | 2010-11-03 | 上海诺德生物实业有限公司 | Method for extracting and producing high content arteannuin |
| CN101899055B (en) * | 2010-08-12 | 2011-05-25 | 湖南农业大学 | Method for rapidly extracting artemisinin |
| CN102453040A (en) * | 2010-10-26 | 2012-05-16 | 曾科 | Process for extracting artemisinin from artemisia apiacea |
| CN102080108A (en) * | 2010-12-15 | 2011-06-01 | 云南弗蓝替生物工程有限公司 | Method for extracting emodin, polydatin and resveratrol from polygonum cuspidatum by using vacuum enzymolysis technology |
| CN102718774B (en) * | 2012-07-10 | 2013-07-03 | 刘志强 | Method for preparing artemisinin |
| CN103059039A (en) * | 2013-01-24 | 2013-04-24 | 湖北民族学院 | Method for extracting artemisine |
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