CN103304576A - Method for extracting artemisinin through enzymatic hydrolysis - Google Patents
Method for extracting artemisinin through enzymatic hydrolysis Download PDFInfo
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- CN103304576A CN103304576A CN201210058448XA CN201210058448A CN103304576A CN 103304576 A CN103304576 A CN 103304576A CN 201210058448X A CN201210058448X A CN 201210058448XA CN 201210058448 A CN201210058448 A CN 201210058448A CN 103304576 A CN103304576 A CN 103304576A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a method for extracting artemisinin. The method comprises the following steps: crushing leaf of Artemisia carvifolia; carrying out enzymatic hydrolysis in an aqueous solution, and carrying out pumping filtration after the enzymatic hydrolysis; carrying out low temperature extraction of the obtained filter cake by using an organic solvent, and concentrating the obtained extract liquid to obtain crude artemisinin; and recrystallizing the crude artemisinin to obtain purified artemisinin. Compared with traditional extraction methods and supercritical extraction methods, the method adopting an enzymatic hydrolysis-reflux two-step extraction technology in the invention has the advantages of simple process, less impurities, low apparatus requirements, and obviously increased extraction rate, and is an environmentally-friendly and efficient artemisinin extraction method. The method is also suitable for extracting sesquiterpene lactones in other medicinal plants.
Description
Technical field
The present invention relates to a kind of extracting method of sesquiterpene lactones, especially a kind of method of from the Chinese medicine sweet wormwood, extracting Artemisinin.
Background technology
Malaria is a kind of global acute parasitic infection that is caused by plasmodium, main torrid areas and the subtropical zone be popular in.In the worldwide, the annual clinical symptom that approximately has 1.5 hundred million people malaria to occur, 1,000,000 to 3,000,000 people are dead because being infected with malaria, and wherein major part is that children and pregnant woman etc. are to the relatively poor crowd of plasmodium immunizing power.
Sweet wormwood is the herb of feverfew Herba Artemisiae annuae (Artemisia annua L.), its contained Artemisinin (Artemisinin) is by China's independent research, and is regarded as the unique effective medicine for the treatment of pernicious malaria by the World Health Organization (WHO).China is the main place of production of sweet wormwood, accounts for more than 90% of global ultimate production, relies on the resources advantage of China's sweet wormwood plantation, carries out the research of extraction technology for artemisia annua element, and is significant to the further industrialization of Artemisinin.
The extracting method of existing Artemisinin mainly contains two kinds of traditional extraction method and supercritical extraction methods, and traditional extraction method comprises reflux extraction, cold soaking extraction method, soxhlet extraction etc.The tradition extraction method extracts repeatedly with organic solvent, and solvent waste is serious, and extraction yield and raw material availability are lower; Though and the supercritical fluid method extraction yield is relatively high, also because of apparatus expensive, universal being extremely restricted.
According to mass transfer theory, in the leaching process of active skull cap components, solvent at first spreads to solid surface, be penetrated into solid surface, then advance dissolving active skull cap components in people's solid interior and the microporosity thereof, spread to solid surface by the solid microporosity at last, and under concentration difference reactive force between solid surface and solvent main body, active skull cap components is finished the extraction mass transfer process to the solvent main diffusion.Because Artemisinin is almost surrounded by the cell walls that Mierocrystalline cellulose consists of, traditional extracting method can't make cell wall rupture, has huge resistance to mass transfer, causes extraction effect not good.Cause the Artemisinin leaf wall to loosen or break by certain physical means or chemical means, will help organic solvent with therefrom stripping of Artemisinin, but the Effective Raise extraction efficiency.
Summary of the invention
This patent provides a kind of extracting method of Artemisinin, take artemisia leaf as main raw material, through first enzymolysis two step process that reflux again, can obtain the Artemisinin of higher degree, and the method has that technique is simple, extraction yield is high and the advantage such as easy amplification preparation.
Technical scheme of the present invention is as follows:
1) with after the artemisia leaf pulverizing, add the aqueous solution and a certain amount of zymin of 2～20 times of weight, the control temperature is 30～60 ℃, thermostatically heating 30min～120min, and cooling is filtered, and filtrate extracts repeatedly with organic solvent, and is for subsequent use after the filter cake cryodrying;
2) toward the organic solvent of 50～100 times of weight of above-mentioned filter cake adding, the control temperature is 30～60 ℃, thermostatically heating 30～120min, and cooling is filtered, filter cake organic solvent repetitive scrubbing, filter cake discards, and filtrate and washings merge;
3) merge 1,2 step gained extraction liquids, washings and filtrate, the sodium hydroxide solution with 2% washs, and washes with water to neutrality again, in 50 ℃ of concentrating under reduced pressure, gets the Artemisinin crude product.Crude product gets the Artemisinin highly finished product through ethyl alcohol recrystallization.
Further, the used aqueous solution is dilution heat of sulfuric acid or dilute hydrochloric acid solution (pH 2～7) in the step 1, and described enzyme is cellulase, and the used enzyme amount of every gram artemisia leaf is 5～20U, and enzymolysis time is for being preferably 30min.
Further, organic solvent is ether or sherwood oil described in the step 1,2, and the add-on of organic solvent is 80 times of artemisia leaf powder weight in the step 2; The step 2 thermostatically heating time is preferably 60min.
The inventive method utilizes cellulase to make the artemisia leaf cell walls loosen, break, and reduces resistance to mass transfer.In addition, enzymolysis can also effectively be removed the impurity such as protein, improves the purity of Artemisinin.Select ether or sherwood oil as extracting solvent, utilize ether or sherwood oil to the Artemisinin good solubility, with Artemisinin stripping the loose microporosity behind enzymolysis, the extraction yield of Effective Raise Artemisinin.
With respect to traditional extraction method and supercritical extraction method, the inventive method has consuming time short, and extraction yield is high, purity is high and the advantage such as low that consumes energy, and is a kind of green and the efficient extracting method of Artemisinin.
According to foregoing, under the prerequisite that does not break away from the above-mentioned basic fundamental thought of the present invention, according to ordinary skill knowledge and the customary means of this area, modification, replacement and the change of various ways can also be arranged to foregoing.
Embodiment
Below in conjunction with specific embodiment content of the present invention is further described:
Embodiment 1
Take by weighing 250g artemisia leaf powder and add in the reaction flask, the cellulase to wherein adding 1L dilution heat of sulfuric acid (pH 6.0) and 2250U places 50 ℃ of waters bath with thermostatic control, behind the enzymolysis 120min, and suction filtration, filter cake is dried to constant weight.Filtrate is used extracted with diethyl ether three times, and extraction liquid is merged.
Add the 2L ether and carry out reflux in above-mentioned filter cake, behind the backflow 120min, be cooled to room temperature, suction filtration, filter cake ether repetitive scrubbing merges above extraction liquid, filtrate and washings, and the sodium hydroxide solution with 2% washs, and washes with water to neutrality again.In 50 ℃ of concentrating under reduced pressure, get the Artemisinin crude product, use at last ethyl alcohol recrystallization, get Artemisinin elaboration 2.07g.
Embodiment 2
Take by weighing 250g artemisia leaf powder and add in the reaction flask, the cellulase to wherein adding 1L dilute hydrochloric acid solution (pH 4.5) and 3750U places 50 ℃ of waters bath with thermostatic control, behind the enzymolysis 30min, and suction filtration, filter cake is dried to constant weight.Filtrate is used petroleum ether extraction three times, and extraction liquid is merged.
Add the 2L sherwood oil and carry out reflux in above-mentioned filter cake, behind the backflow 60min, be cooled to room temperature, suction filtration, filter cake sherwood oil repetitive scrubbing merges above extraction liquid, filtrate and washings, and the sodium hydroxide solution with 2% washs, and washes with water to neutrality again.In 50 ℃ of concentrating under reduced pressure, get the Artemisinin crude product, use at last ethyl alcohol recrystallization, get Artemisinin elaboration 2.911g.
Embodiment 3
Take by weighing 250g artemisia leaf powder and add in the reaction flask, the cellulase to wherein adding 1L dilution heat of sulfuric acid (pH 3.0) and 3750U places 50 ℃ of waters bath with thermostatic control, behind the enzymolysis 120min, and suction filtration, filter cake is dried to constant weight.Filtrate is used petroleum ether extraction three times, and extraction liquid is merged.
Add the 1.5L sherwood oil and carry out reflux in above-mentioned filter cake, behind the backflow 30min, be cooled to room temperature, suction filtration, filter cake ether repetitive scrubbing merges above extraction liquid, filtrate and washings, and the sodium hydroxide solution with 2% washs, and washes with water to neutrality again.In 50 ℃ of concentrating under reduced pressure, get the Artemisinin crude product, use at last ethyl alcohol recrystallization, get Artemisinin elaboration 2.48g.
Embodiment 4
Take by weighing 250g artemisia leaf powder and add in the reaction flask, the cellulase to wherein adding 1L dilute hydrochloric acid solution (pH 4.0) and 5250U places 50 ℃ of waters bath with thermostatic control, behind the enzymolysis 60min, and suction filtration, filter cake is dried to constant weight.Filtrate is used extracted with diethyl ether three times, and extraction liquid is merged.
Add the 2L ether and carry out reflux in above-mentioned filter cake, behind the backflow 30min, be cooled to room temperature, suction filtration, filter cake ether repetitive scrubbing merges above extraction liquid, filtrate and washings, and the sodium hydroxide solution with 2% washs, and washes with water to neutrality again.In 50 ℃ of concentrating under reduced pressure, get the Artemisinin crude product, use at last ethyl alcohol recrystallization, get Artemisinin elaboration 2.31g.
The specific implementation method of more than showing by the embodiment form is described in further detail summary of the invention.But this should be interpreted as that the scope of theme of the present invention only limits to following example.All technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Claims (7)
1. the extracting method of an Artemisinin is characterized in that may further comprise the steps:
1) with after the artemisia leaf pulverizing, add the aqueous solution and a certain amount of zymin of 2～20 times of weight, the control temperature is 30～60 ℃, thermostatically heating 30min～120min, and cooling is filtered, and filtrate extracts repeatedly with organic solvent, and is for subsequent use after the filter cake cryodrying;
2) toward the organic solvent of 50～100 times of weight of above-mentioned filter cake adding, the control temperature is 30～60 ℃, thermostatically heating 30～120min, and cooling is filtered, filter cake organic solvent repetitive scrubbing, filter cake discards, and filtrate and washings merge;
3) merge 1,2 step gained extraction liquids, washings and filtrate, the sodium hydroxide solution with 2% washs, and is washed till neutrality with distilled water, in 50 ℃ of concentrating under reduced pressure, gets the Artemisinin crude product.Crude product gets the Artemisinin highly finished product through ethyl alcohol recrystallization.
2. the extracting method of Artemisinin as claimed in claim 1 is characterized in that the described aqueous solution is dilution heat of sulfuric acid or dilute hydrochloric acid solution, and the pH value is 2～7.
3. the extracting method of Artemisinin as claimed in claim 2 is characterized in that described enzyme is cellulase, and the enzyme dosage of 1 gram artemisia leaf powder is 5～20U.
4. the extracting method of Artemisinin as claimed in claim 3 is characterized in that enzymolysis time is 30min in the step 1.
5. the extracting method of Artemisinin as claimed in claim 4 is characterized in that the organic solvent that uses in the step 1,2 is ether or sherwood oil.
6. the extracting method of Artemisinin as claimed in claim 5 is characterized in that solid-liquid ratio is 1: 80 in the step 2.
7. the extracting method of Artemisinin as claimed in claim 6 is characterized in that the thermostatically heating time is 60min in the step 2.
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| CN201210058448XA CN103304576A (en) | 2012-03-07 | 2012-03-07 | Method for extracting artemisinin through enzymatic hydrolysis |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327091A (en) * | 2013-11-30 | 2015-02-04 | 钟延华 | Extraction method for artemisinin |
| CN104497002A (en) * | 2013-12-05 | 2015-04-08 | 广西仙草堂制药有限责任公司 | Extraction method of artemisinin |
| CN107522708A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of production technology of enzymatic isolation method extraction qinghaosu |
| CN107857770A (en) * | 2017-12-25 | 2018-03-30 | 禹州市天源生物科技有限公司 | A kind of method of enzymolysis and extraction qinghaosu |
| CN108299461A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | A kind of qinghaosu extracting method of environment-friendly high-efficiency |
| CN108299460A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | The environment-friendly high-efficiency extracting method of qinghaosu and Artemisitene |
| CN111838624A (en) * | 2020-07-28 | 2020-10-30 | 上海金山德乐食品配料有限公司 | Method for extracting natural oat sesquiterpene and monoterpene compounds |
| CN115153020A (en) * | 2022-07-29 | 2022-10-11 | 武汉橙炻科技有限公司 | Medicinal and edible food capable of efficiently removing harmful free radicals from human body and preparation method of medicinal and edible food |
-
2012
- 2012-03-07 CN CN201210058448XA patent/CN103304576A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327091A (en) * | 2013-11-30 | 2015-02-04 | 钟延华 | Extraction method for artemisinin |
| CN104497002A (en) * | 2013-12-05 | 2015-04-08 | 广西仙草堂制药有限责任公司 | Extraction method of artemisinin |
| CN107522708A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of production technology of enzymatic isolation method extraction qinghaosu |
| CN107857770A (en) * | 2017-12-25 | 2018-03-30 | 禹州市天源生物科技有限公司 | A kind of method of enzymolysis and extraction qinghaosu |
| CN108299461A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | A kind of qinghaosu extracting method of environment-friendly high-efficiency |
| CN108299460A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | The environment-friendly high-efficiency extracting method of qinghaosu and Artemisitene |
| CN108299461B (en) * | 2018-03-21 | 2019-09-27 | 黑龙江赛美生物科技开发有限公司 | A kind of qinghaosu extracting method |
| CN108299460B (en) * | 2018-03-21 | 2019-11-01 | 四川协力制药股份有限公司 | The extracting method of qinghaosu and Artemisitene |
| CN111838624A (en) * | 2020-07-28 | 2020-10-30 | 上海金山德乐食品配料有限公司 | Method for extracting natural oat sesquiterpene and monoterpene compounds |
| CN111838624B (en) * | 2020-07-28 | 2023-04-07 | 上海金山德乐食品配料有限公司 | Method for extracting natural oat sesquiterpene and monoterpene compounds |
| CN115153020A (en) * | 2022-07-29 | 2022-10-11 | 武汉橙炻科技有限公司 | Medicinal and edible food capable of efficiently removing harmful free radicals from human body and preparation method of medicinal and edible food |
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Application publication date: 20130918 |