CN1108303C - Microwave extracting method of artemisine - Google Patents
Microwave extracting method of artemisine Download PDFInfo
- Publication number
- CN1108303C CN1108303C CN 00120351 CN00120351A CN1108303C CN 1108303 C CN1108303 C CN 1108303C CN 00120351 CN00120351 CN 00120351 CN 00120351 A CN00120351 A CN 00120351A CN 1108303 C CN1108303 C CN 1108303C
- Authority
- CN
- China
- Prior art keywords
- microwave
- extracting method
- extraction
- described extracting
- 2450mhz
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The present invention discloses a new method for extracting artemisinin from a crushed material of artemisia annua plants. In the method, the crushed material of the artemisia annua plants is processed by microwaves whose frequency is 2450MHz or 915MHz and power is from 500 to 15000 W in a solvent selected from water, alcohol of C1 to C4, ether, acetone or a mixture thereof. Compared with the conventional chemical method, the method of the present invention has the advantages of simple and convenient technology, high efficiency, high speed, low cost and small discharge amount of waste liquid.
Description
Present invention relates in general to separation, the extraction of material, more particularly, the present invention relates to from the sweet wormwood plant particle, extract the method for Artemisinin with microwave radiation.
The Artemisinin that is present in the sweet wormwood plant particle is useful active constituents of medicine.Artemisinin is a class new antimalarial agent.At present, Artemisinin generally is from feverfew Herba Artemisiae annuae (Artemisia
At present, the method for extracting Artemisinin from the sweet wormwood plant particle has two big classes basically, and the one, the traditional chemical solvent extraction method, another kind of is the supercritical extraction method.Yet this two classes extraction process all exists many defectives.
Particularly, the shortcoming of chemical solvents extraction has the energy, raw materials consumption amount big, and extraction efficiency is not high, and the industrial pollution quantity discharged is big etc.For example, CN1092073A discloses with ethanol, has contained the method that the industrial naptha of benzene or ethyl acetate carries out lixiviate to chrysanthemum mugwort powder.The yield of this method is about 0.45%.
In addition, the someone discloses with the supercritical extraction method and has extracted Artemisinin.For example, CN1095381A discloses a kind of method of utilizing supercritical co extracting and separating Artemisinin from the sweet wormwood plant particle.From the Figure of description of this application, as seen, then need CO for implementing this method
2A series of equipment such as gas bottle, compression pump, heat exchanger, extraction kettle, resolver, cooling reactor, and need under certain pressure (extracting pressure is the 8-32 MPa, and resolving pressure is the 4-8 MPa), to carry out.Make that this extraction cost is higher, and the equipment that these class methods require is complicated, the solvent range of choice is narrow, is unfavorable for scale operation.As seen, these class methods also exist certain defective.
Because microwave extracting can carry out the selectivity heating to the different components in the extraction system, and because microwave is to utilize molecular polarization or ionic conduction effect and directly material is heated, therefore can make that target components is easier dissociates out from extract, and the thermo-efficiency height has improved extraction efficiency.Yet up to this point, still nobody adopts microwave to extract Artemisinin.
The objective of the invention is to overcome the shortcoming that exists in the prior art,, provide the novel method of from the sweet wormwood plant particle, extracting Artemisinin fast and efficiently by utilizing the characteristics of microwave extracting.That is, provide a kind of and can replace the simple and easy to do, efficient, quick of above-mentioned traditional solvent lixiviate and supercritical fluid extraction technology, cost is low, the novel method that the discharging of waste liquid amount is few.
The present invention is that to adopt frequency be that 2450MHz or 915MHz, power are that 500-15000 watt microwave is handled in solvent the sweet wormwood plant particle, extracts the novel method of Artemisinin from the sweet wormwood plant particle.
Particularly, the present invention includes following aspect:
The invention provides a kind of extracting method of Artemisinin, this method comprises:
With frequency is that 2450MHz or 915MHz, power are that 500-15000 watt microwave is being selected from water, C to the sweet wormwood plant particle
1-C
4The solvent of alcohol, ether, acetone or its mixture in the microwave treatment step handled.
In above-mentioned extracting method, preferred used microwave frequency is 2450MHz, and microwave treatment time is 1-30 minute.
In above-mentioned extracting method, preferred described microwave treatment is divided and is carried out for 1-3 time, each 1-10 minute.
In above-mentioned extracting method, the amount of preferred described solvent and sweet wormwood plant particle is counted 6-8 by weight: 1.
In above-mentioned extracting method, preferred described sweet wormwood plant particle is a form in small, broken bits, and particle diameter is smaller or equal to 5 millimeters.
In above-mentioned extracting method, preferably also be included in after the described microwave treatment, with being selected from industrial naptha, sherwood oil, C
1-C
3The step that the extraction liquid of alcohol and composition thereof extracts once more to the first extract of microwave extraction gained.
In above-mentioned extracting method, preferred describedly extract once more that to adopt frequency be that 2450MHz or 915MHz power are that 500-15000 watt microwave carries out.
In above-mentioned extracting method, preferred described microwave treatment is divided and is carried out for 1-3 time, each 1-5 minute.
In above-mentioned extracting method, preferably the first extract of microwave extraction gained is concentrated, and then count 1 by weight with extraction liquid: 4-8 mixes.
The present invention also randomly be included in carry out described extract once more before, the first extract that will be from the sweet wormwood plant particle obtains through 1-30 minute, preferred 1-20 minute preliminary microwave extraction concentrates and reclaims solvent.The present invention carries out purifying with recrystallization method, active carbon adsorption and chromatography column method with isolated refining liquid after also randomly being included in above-mentioned smart once more the extraction after concentrated.Then, the crude product behind the purifying is carried out concentrate drying, get artemislnin content at the product more than 95%.
The sweet wormwood plant particle that the present invention adopts comprises the particle of chrysanthemum straw and leaf, and the chrysanthemum mugwort particle of preferably gathering recently, more preferably will described fresh sweet wormwood plant particle pulverizing be not more than 5 millimeters or grind to form the sweet wormwood plant slurry for diameter.For the not restriction more especially of degree in small, broken bits of above-mentioned particle, but in general be more in small, broken bits good more.
It extraction container of the present invention is had no particular limits, as long as can be used for microwave heating.This container can be open, also can have lid.Its example has the extractor of glass beaker, extractor such as tetrafluoroethylene or ceramic inner walls etc.
The microwave frequency that the present invention adopts is 2450MHz or 915MHz.The frequency of most industrial or civilian microwave instrument is 2450MHz at present.The inventor thinks that another industrial microwave frequency 915MHz also can realize purpose of the present invention.This be because the wavelength of 915MHz microwave greater than the wavelength of 2450MHz microwave, its to the penetration coefficient of vegetable cell should microwave unlike 2450MHz a little less than, and the final output rating of two kinds of microwaves can be adjusted to certain value, therefore, as long as coordinate the microwave output parameter, 915MHz is suitable for equally and extracts.2450MHz is the preferred frequency of the present invention.The power of the used microwave apparatus of the present invention is 500-15000 watt or bigger, preferred 500-15000 watt.
Carry just at the microwave of the inventive method that adoptable extraction agent is a water in the step, C
1-C
4Alcohol is as methyl alcohol, ethanol, propyl alcohol etc., ether, acetone, ethyl acetate etc.In preliminary extraction step of the present invention, solvent for use is preferably water, methyl alcohol, ethanol, ether and acetone etc., and they can use separately, also can mix use.(abbreviate as solid: liquid)=1: 4-10 is preferably 6-8 to the ratio (weight ratio) of used sweet wormwood plant particle and extraction agent.The microwave radiation processing time of this step is 1-20 minute, preferred 10-15 minute.This microwave is just put forward step and can be divided and carry out for 1-3 time, each microwave action 1-10 minute.
Extract in (essence is carried) step once more of the present invention, spendable solvent is preferably industrial naptha, sherwood oil and ethanol etc., and they can use separately, also can mix use.Wherein will just carry the enriched material that concentrates gained after the step and this extraction agent by 1: the mixed of 4-8 (volume ratio).Above-mentioned smart extraction step can be the traditional extraction step, also can be the microwave extracting step as the thick extraction step of the present invention, and the latter is preferred.When extracting once more with microwave treatment, this microwave treatment can be 1-15 minute, preferably divides and carries out for 1-3 time, each 1-5 minute.
After finishing above-mentioned essence and carrying, the inventive method also randomly concentrates the refining liquid of gained, and removes look and decon with the solvent that is selected from ethanol, acetoneand ethyl acetate of 1-3 times of volume and the gac that is equivalent to Herba Artemisiae annuae particle 1-4%.Certainly, the purpose of this step also can realize that these are that those of ordinary skill in the art is known by making refining liquid cross polyamide resin column or recrystallization and centrifugal mode.
Therefore, more particularly, particularly preferred method of the present invention comprises the steps: that with being crushed to particle diameter be that sweet wormwood plant particle below 5 millimeters is solid: the ratio of liquid=1: 6-8 be selected from water, C
1-C
4The solvent of alcohol, ether, acetone or its mixture mix, be that 2450MHz, power tentatively add extraction heat 10-15 minute at 500-15000 watt microwave apparatus with frequency then, filter to isolate extract just then, behind concentrating under reduced pressure, be 1 by volume in resistates: the ratio adding of 4-8 is selected from industrial naptha, sherwood oil, C
1-C
3The extraction liquid of alcohol and composition thereof, equally, with frequency is 2450MHz power at 500-15000 watt microwave apparatus to gained mixture effect 1-10 minute, then filter and concentrate, the gac that adds 1-3 times of volume of ethanol, ethyl acetate or acetone and 1-4%, after the agitation and filtration, with supernatant liquor concentrating under reduced pressure, dry to make the product of the inventive method.
Be the higher Artemisinin goods of preparation purity, also available about 70% ethanol or acetone dissolve the product of the invention described above, and wash with water 1-3 time, and then through concentrating under reduced pressure, drying, can make artemislnin content at the goods more than 98%.
With the artemislnin content in the high-efficient liquid phase color spectrometry products therefrom.
From as can be seen above-mentioned, the inventive method step is easy, easy handling.In addition, the extraction efficiency of the inventive method also greatly reduces the content of non-target component also than higher.
In the mode of embodiment, the present invention is done more detailed description below.
Embodiment 1:
To give birth to sweet wormwood plant then and comprise that bar and leaf are crushed to particle diameter smaller or equal to 5 millimeters, particle 1.0kg is packed in 2 liters the glass beaker, add entry: ethanol: the solvent of ether=40: 55: 5 (volume ratio), Gu: liquid (weight ratio)=1: 8, with power is microwave oven (the National K577 WFS that 1000 watts of frequencies are 2540MHz, 1300W, 6A) heating was extracted 30 minutes, removed residue after filtration, behind the concentrating under reduced pressure, get extract 2kg just, use petrolic solvent again: ethanol=70: 30 (volume ratio) mixed solvent 6.5kg, extracted 2 hours in room temperature is smart with extraction process routinely, separate and concentrate through separating funnel, to the ethyl acetate 5kg and 5% gac that wherein add 75%, stir, filter, concentrate, and with behind 75% the acetone solution, again through separating, concentrate, drying under reduced pressure get final product product 4.5g.The content of surveying Artemisinin with high efficiency liquid chromatography is 98%.
Wherein the parameter of used high efficiency liquid chromatography is as follows:
Chromatographic column: C18
Eluent: methyl alcohol 70%
Elution rate: 1.0ml/min
Wavelength: 290nm
Embodiment 2:
The sweet wormwood plant particle 1kg of chopping is packed in the extractor, add sherwood oil: ethanol: the solvent of water=0.7: 0.2: 0.1, Gu: liquid=1: 6 is the extracting through microwave heating 15 minutes of 2450MHz for the 6000W frequency with power, separate through filtration under diminished pressure, reclaim first extract.Use petrolic solvent again: ethanol=70: 30 (volume ratio) mixed solvent extracts, wherein, through stirring, extracted 1.5 hours more earlier with the microwave action identical with power 5 minutes with just putting forward the used frequency of step, separate after filtration, concentrate, carry out recrystallization and remove look, filter with 70% ethyl acetate and 3% gac, concentrate, behind 75% dissolve with ethanol, through separating concentrating under reduced pressure, the dry product 5.1g that gets.Wherein the content with high efficiency liquid chromatography survey Artemisinin is 97%.Condition determination is with embodiment 1.
Embodiment 3
Press the mode of embodiment 2, carry out the extraction of Artemisinin, just microwave among the embodiment 2 is just carried used extraction liquid is replaced by water: acetone=40: 60, microwave is extracted used extraction liquid once more be replaced by sherwood oil: ethyl acetate=70: 30, carry out recrystallization with 80% ethanol in the purification step.Get product 4.1, artemislnin content is 99%.
Comparative example
Adopt sweet wormwood plant particle 100 grams, experimentize with method and the common extraction process of embodiment 1.Difference of these two experiments only is that common extraction process is to replace the microwave among the embodiment 1 just to carry in 30 minutes with 1000 watts electric furnace heating and refluxing extraction.As a result, adopt the electric furnace heating and refluxing extraction, get product 0.87g, artemislnin content is 37%.
In sum, the present invention passes through to adopt microwave, and is equipped with appropriate solvent, can extract Artemisinin from the sweet wormwood plant particle fast and efficiently.The energy of technology of the present invention, solvent consumption are saved 70-90% than conventional chemical solvent soaking extraction process, and the discharging of waste liquid amount reduces about 80-90%, belongs to typical clean environment production technique.
Claims (9)
1. the extracting method of an Artemisinin, this method comprises:
With frequency is that 2450MHz or 915MHz, power are that 500-15000 watt microwave is being selected from water, C to the sweet wormwood plant particle
1-C
4The solvent of alcohol, ether, acetone or its mixture in the microwave treatment step handled.
2. the described extracting method of claim 1, wherein used microwave frequency is 2450MHz, microwave treatment time is 1-30 minute.
3. the described extracting method of claim 2, wherein said microwave treatment divide and carry out each 1-10 minute for 1-3 time.
4. each described extracting method among the claim 1-3, the amount of wherein said solvent and sweet wormwood plant particle is counted 6-8 by weight: 1.
5. each described extracting method among the claim 1-3, wherein said sweet wormwood plant particle are form in small, broken bits, and particle diameter is smaller or equal to 5 millimeters.
6. the described extracting method of claim 1 also has been included in after the described microwave treatment, with being selected from industrial naptha, sherwood oil, C
1-C
3The step that the extraction liquid of alcohol and composition thereof extracts once more to the first extract of microwave extraction gained.
7. the described extracting method of claim 6 describedly extracts once more that to adopt frequency be that 2450MHz or 915MHz power are that 500-15000 watt microwave carries out.
8. the described extracting method of claim 7, wherein said microwave treatment divide and carry out each 1-5 minute for 1-3 time.
9. each described extracting method among the claim 6-8, wherein the microwave extraction gained just extract and used extraction liquid count 1 by weight: 4-8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00120351 CN1108303C (en) | 2000-07-08 | 2000-07-08 | Microwave extracting method of artemisine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00120351 CN1108303C (en) | 2000-07-08 | 2000-07-08 | Microwave extracting method of artemisine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1281859A CN1281859A (en) | 2001-01-31 |
| CN1108303C true CN1108303C (en) | 2003-05-14 |
Family
ID=4588175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00120351 Expired - Fee Related CN1108303C (en) | 2000-07-08 | 2000-07-08 | Microwave extracting method of artemisine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1108303C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103054924A (en) * | 2012-12-29 | 2013-04-24 | 黄家芬 | Extraction method of artemisia annua extract |
| CN103509034B (en) * | 2013-09-29 | 2016-06-08 | 重庆市中药研究院 | A kind of method extracting arteannuin from fresh artemisia annua |
| CN104031062A (en) * | 2014-06-30 | 2014-09-10 | 施佩蓓 | Method for producing artemisinin |
-
2000
- 2000-07-08 CN CN 00120351 patent/CN1108303C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1281859A (en) | 2001-01-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101492483B (en) | Method for extraction and purification of cordycepin, and method for preparation of cordycepin dry powder | |
| CN101973984B (en) | Method for extracting general flavones from bamboo leaves | |
| CN102617316B (en) | Method for extracting curcumin from turmeric | |
| CN101703635B (en) | Production technology of grape pip and grape skin extract | |
| CN109135807A (en) | A kind of high-efficient demulsifier | |
| CN1102589C (en) | Microwave extraction method of protocyaidin-like substances from grape seed | |
| CN107936265B (en) | Method for extracting plant condensed tannin polymer | |
| CN1108303C (en) | Microwave extracting method of artemisine | |
| CN1109028C (en) | Microwave extraction method of ginkgolic flavone and bilobalide-like substances | |
| CN1321735A (en) | Method for extracting onion oil | |
| CN1363365A (en) | Extraction of herbs by heating alcohol | |
| KR102187312B1 (en) | The tub glycerine extractor of the glycerine containing waste and method and the tub glycerine extracted to the method thereof | |
| CN107812510A (en) | A kind of composite type water treating agent and preparation method thereof | |
| CN1141267C (en) | Process for treating oily mud by phase transfer method | |
| CN1279010C (en) | Method of high effect preparing tea polyphenol | |
| CN1107075C (en) | Microwave process of extracting polysaccharides and polyphenols from tea | |
| CN111925408B (en) | Preparation method of periplaneta americana polypeptide extract taking water as medium | |
| CN102079883B (en) | Novel process for extracting capsanthin and chilli extract by composite solvent | |
| CN1246316C (en) | Method for separating major monomeric compoent of soybean isoflavone | |
| CN107759467A (en) | A kind of preparation method for improving carnosic acid content in rosemary fat-soluble antioxidant | |
| CN110066256B (en) | Purification method of 5-chloro-2-methyl-4-isothiazolin-3-one | |
| RU2279284C1 (en) | Method for integrated utilization of larch wood | |
| CN1483734A (en) | Novel process for extracting puerarin from pueraria mirifica | |
| JP2017071569A (en) | Method of extracting condensation type tannin high in polymerization degree | |
| CN110585339A (en) | Method for separating and preparing multiple effective components of bletilla striata |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |