CN103664987A - Artemisinin and preparation method thereof - Google Patents
Artemisinin and preparation method thereof Download PDFInfo
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- CN103664987A CN103664987A CN201310725567.0A CN201310725567A CN103664987A CN 103664987 A CN103664987 A CN 103664987A CN 201310725567 A CN201310725567 A CN 201310725567A CN 103664987 A CN103664987 A CN 103664987A
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- C07—ORGANIC CHEMISTRY
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- 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
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Abstract
The invention discloses a preparation method for artemisinin. The method comprises the following steps: (1) drying and smashing artemisia apiacea as a medical raw material into powder of 20-80 meshes; (2) performing reflux extraction twice on the material, combing extracting solutions generated from the two reflux extractions and concentrating for standby, wherein ethyl acetate is used as a solvent, and intermittent vacuumizing and vacuum breaking are performed on an extracting tank during extracting process; (3) adsorbing a concentrated artemisinin extracting solution by using macroporous resin with moderate polarity, eluting the concentrated artemisinin extracting solution by using 90-99.7% of alcohol, concentrating and crystallizing an eluate, recrystallizing with 50-90% of alcohol, and drying to obtain an artemisinin product. According to the invention, through the combination between pulsating vacuum extraction and adsorption of macroporous resin, the production with low cost and high efficiency for preparing the artemisinin from the artemisia apiacea is realized and the market application prospect is wide.
Description
Technical field
The present invention relates to a kind of preparation method of Artemisinin, specifically refer to extract the method for artemisinin purifying from Chinese medicinal materials sweet wormwood.
Background technology
Artemisinin is the sesquiterpene lactones new antimalarial agent that has peroxy-radical extracting from Chinese medicine sweet wormwood, synthesized on its basis multiple derivative, as dihydroarteannuin, Artemether, Artesunate etc., artemisinin-based drug because toxicity is low, anti-cruel property is strong, thereby has very important pharmaceutical use.
Artemisinin is colourless acicular crystal, bitter, be soluble in acetone, vinyl acetic monomer, chloroform, in the weak organic solvent of benzene and sherwood oil isopolarity, thereby from sweet wormwood, extract Artemisinin and generally all adopt 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, these solvents are poor to the penetrance of strong polarity and hydroaropic substance, Artemisinin be take again the plant cell tissue that Mierocrystalline cellulose and pectin is main component and is wrapped up, thereby there is very large resistance to mass transfer in these solvents in leaching process, solvent is difficult to remove to dissolve Artemisinin through plant cell tissue, the solution that has 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, in leaching process, also bring a large amount of impurity thereupon, thereby need to carry out purifying, purifying process present stage mainly adopts silica gel column chromatography, but silica gel column chromatography exists the shortcoming that yield is low, cost is high, thereby prior art can not meet the requirement that Artemisinin is produced.
Summary of the invention
The problem existing for solving the above-mentioned prior art of extracting Artemisinin from sweet wormwood, the 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) processing of raw medicinal material: raw medicinal material sweet wormwood is dried and is crushed to 20-80 order.
(2) extraction of Artemisinin: the ethyl acetate of take is carried out refluxing extraction twice to material as solvent, during extraction, solvent is with the volume mass of material than being 2:1-12:1, and extraction time 1-5 hour, merges extracted twice liquid concentrated, standby.Volume mass than in the unit of volume be milliliter that the unit of quality is gram.
In said extracted process, extractor is carried out to step vacuumizing and vacuum breaker, utilize vacuum pulsation reinforcing mass transfer.The mechanism of vacuum pulsation reinforcing mass transfer is: because ethyl acetate is the weakly polar organic solvent that volatility is stronger, ethyl acetate while 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 in sweet wormwood histocyte and presses, ethyl acetate outside sweet wormwood histocyte enters rapidly sweet wormwood histocyte inside and removes to dissolve Artemisinin because of differential pressure action, alternately changing and strengthened solvent and be dissolved in the Artemisinin mass transfer in solvent of this sweet wormwood histocyte external and internal pressure, reduces extraction efficiency raising, 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%, after dry, obtain Artemisinin product, in product, the massfraction of Artemisinin can reach 99.5%-99.99%.
After wash-out completes, continue can realize the activation of macroporous adsorbent resin and reuse, general reusable 3-5 time of resin with ethanol elution for some time of 90-99.7%.
Compared with prior art, the invention has the beneficial effects as follows: extractor is carried out to step vacuumizing and vacuum breaker, adopt vacuum pulsation reinforcing mass transfer, effectively shortened extraction time, improved the extraction yield of Artemisinin; When adopting vacuum pulsating be extracted in shortening extraction time and guarantee extraction yield, also reduced the requirement to equipment, common refluxing extraction tank can be realized through simple transformation, has reduced cost; The purifying of Artemisinin adopts the ethanol elution of semipolar absorption with macroporous adsorbent resin, high density, and the use of macroporous resin and activation one step are completed, and has reduced operation steps, has reduced cost.
In sum, the present invention is by organically combining the extraction of vacuum pulsating and macroporous resin adsorption, low cost and the High-efficient Production of from sweet wormwood, extracting separated Artemisinin have been realized, through evidence, use this technique to extract Artemisinin separated, product yield can improve 3%-5%, cost 5%-8%, and market application foreground is wide.
Embodiment
Below the preparation method of Artemisinin is elaborated.
Embodiment 1:
(1) processing of raw medicinal material: raw medicinal material sweet wormwood is dried and is crushed to 25 orders.
(2) extraction of Artemisinin: the ethyl acetate of take is carried out refluxing extraction twice to material as solvent, during extraction, solvent is 3:1 with the volume mass ratio of material, 4.5 hours extraction times, merge extracted twice liquid concentrated, standby, volume mass than in the unit of volume be milliliter that the unit of quality is gram, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker, utilize vacuum pulsation reinforcing mass transfer.
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then 91% ethanol carries out wash-out, elutriant is through the ethyl alcohol recrystallization of concentrated, crystallization and 60%, obtains Artemisinin product after dry, and in product, the massfraction of Artemisinin is 99.58%.
After wash-out completes, continue to realize with ethanol elution for some time of 95% activation of macroporous adsorbent resin.
Embodiment 2:
(1) processing of raw medicinal material: raw medicinal material sweet wormwood is dried and is crushed to 40 orders.
(2) extraction of Artemisinin: the ethyl acetate of take is carried out refluxing extraction twice to material as solvent, during extraction, solvent is 6:1 with the volume mass ratio of material, 3 hours extraction times, merge extracted twice liquid concentrated, standby, volume mass than in the unit of volume be milliliter that the unit of quality is gram, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker, utilize vacuum pulsation reinforcing mass transfer.
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then 95% ethanol carries out wash-out, elutriant is through the ethyl alcohol recrystallization of concentrated, crystallization and 75%, obtains Artemisinin product after dry, and in product, the massfraction of Artemisinin is 99.75%.
After wash-out completes, continue to realize with ethanol elution for some time of 92% activation of macroporous adsorbent resin.
Embodiment 3:
(1) processing of raw medicinal material: raw medicinal material sweet wormwood is dried and is crushed to 70 orders.
(2) extraction of Artemisinin: the ethyl acetate of take is carried out refluxing extraction twice to material as solvent, during extraction, solvent is 10:1 with the volume mass ratio of material, 1.5 hours extraction times, merge extracted twice liquid concentrated, standby, volume mass than in the unit of volume be milliliter that the unit of quality is gram, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker, utilize vacuum pulsation reinforcing mass transfer.
(3) purifying of Artemisinin: by the semipolar absorption with macroporous adsorbent resin of Artemisinin extracting solution after concentrated, then 99% ethanol carries out wash-out, elutriant is through the ethyl alcohol recrystallization of concentrated, crystallization and 88%, obtains Artemisinin product after dry, and in product, the massfraction of Artemisinin is 99.91%.
After wash-out completes, continue to realize with ethanol elution for some time of 98% activation of macroporous adsorbent resin.
Claims (3)
1. a preparation method for Artemisinin, is characterized in that comprising following step:
(1) processing of raw medicinal material: raw medicinal material sweet wormwood is dried and is crushed to 20-80 order;
(2) extraction of Artemisinin: the ethyl acetate of take is carried out refluxing extraction twice to material as solvent, during extraction, solvent is 2:1-12:1 with the volume mass ratio of material, extraction time 1-5 hour, merge extracted twice liquid concentrated, standby, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker;
(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, through the ethyl alcohol recrystallization of concentrated, crystallization and 50-90%, obtains Artemisinin product after being dried.
2. the preparation method of Artemisinin according to claim 1, is characterized in that: the ethanol elution of 90-99.7% for continuation after wash-out completes, realize the activation of macroporous adsorbent resin.
3. the Artemisinin product that the preparation method of Artemisinin obtains according to claim 1, is characterized in that: in product, the massfraction of Artemisinin is 99.5%-99.99%.
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| CN201310725567.0A CN103664987B (en) | 2013-12-25 | 2013-12-25 | Artemisinin and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108299459A (en) * | 2018-03-16 | 2018-07-20 | 中国科学院过程工程研究所 | A kind of method of polyethylene glycols solvent extraction qinghaosu |
| CN114271533A (en) * | 2022-02-14 | 2022-04-05 | 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108299459A (en) * | 2018-03-16 | 2018-07-20 | 中国科学院过程工程研究所 | A kind of method of polyethylene glycols solvent extraction qinghaosu |
| CN114271533A (en) * | 2022-02-14 | 2022-04-05 | 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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| CN103664987B (en) | 2016-01-20 |
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