CN107312015A - A kind of technique of efficiently extracting and producing artemisinin by ionic liquid - Google Patents
A kind of technique of efficiently extracting and producing artemisinin by ionic liquid Download PDFInfo
- Publication number
- CN107312015A CN107312015A CN201710472851.XA CN201710472851A CN107312015A CN 107312015 A CN107312015 A CN 107312015A CN 201710472851 A CN201710472851 A CN 201710472851A CN 107312015 A CN107312015 A CN 107312015A
- Authority
- CN
- China
- Prior art keywords
- qinghaosu
- ionic liquid
- liquid
- extract solution
- crude product
- 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.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Compounds Of Unknown Constitution (AREA)
Abstract
The present invention relates to a kind of technique of efficiently extracting and producing artemisinin by ionic liquid, comprise the following steps：1) dry sweet wormwood blade of grass is carried out being crushed to powder；2）Sweet Wormwood Herb was subjected to 90 mesh sieves, compares 2 by solid-liquid:7‑2:80 add the mixed liquor of glyoxaline ion liquid halide salts and water, in the 100W/cm of ultrasonic power 12, the 80kHz of supersonic frequency 20 under the conditions of 20 60 DEG C of temperature, extracts 70 minutes, the extract solution containing qinghaosu obtained through solid-liquor separation；3）By step 2) obtained extract solution extracts 6 times by qinghaosu extract solution, and separation organic phase obtains qinghaosu extraction phase, and raffinate phase ionic liquid is recycled；4）By step 3) obtained organic extraction mutually evaporates after recovery organic extractant to obtain qinghaosu crude product；5）By step 4) obtained qinghaosu crude product is redissolved, further be refining to obtain high-purity qinghaosu with column chromatography, recrystallization, there is the present invention extractant not fire, it is non-volatile, be lost it is small, consume energy it is low, without potential safety hazard, it is easy to operate, be easy to industrialized advantage.
Description
Technical field
The invention belongs to qinghaosu preparation technology field, and in particular to a kind of efficiently extracting and producing artemisinin by ionic liquid
Technique.
Background technology
Qinghaosu is that a kind of obtained colourless acicular crystal is extracted from compound inflorescence plant Artemisia annua i.e. Chinese medicine artemisia leaf,
Not pastille sweet wormwood in its stem, qinghaosu is the maximally effective antimalarial specific drug after pyrimethamine, chloroquine, primary quinoline, especially
For encephalic malaria and anti-chlorine quinoline malaria, the characteristics of with quick-acting and low toxicity, once it was referred to as " in the world only by the World Health Organization
One effective malaria treatment medicine "；The anti-malarial mechanism of action is essentially consisted in passes through qinghaosu activation production in the process for treating malaria
Raw free radical, free radical and the former protein binding of malaria, act on the film structure of plasmodium, make its vacuolar membrane, nuclear membrane and plasma membrane equal
Destroyed, mitochondrial swelling, interior outer membrane comes off, so that the eucaryotic cell structure and its function to plasmodium are damaged；In addition it is blue or green
Punt-pole element also shows that tempting prospect in the treatment of other diseases；Such as immunologic function of anti-schistosome, regulation or suppression body fluid,
The conversion ratio of lymphocyte is improved, cholagogic, eliminating the phlegm, antibechic is relievingd asthma, therefore qinghaosu has great medical market prospect；
Existing qinghaosu is extracted uses volatile organic solvent mostly, although can significantly shorten extraction time, but volatility
Organic solvent can produce the problem of safety and environmental pollution unavoidably, it is therefore necessary to the extracting method to qinghaosu changes
Enter.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, and it is blue or green to provide a kind of ionic liquid high efficiency extraction production
The technique of artemisin.
The object of the present invention is achieved like this：A kind of technique of efficiently extracting and producing artemisinin by ionic liquid, including such as
Lower step：
1) dry sweet wormwood blade of grass is carried out being crushed to powder；
2）Sweet Wormwood Herb was subjected to 90 mesh sieves, compares 2 by solid-liquid:7-2:80 add glyoxaline ion liquid halide salts and water
Mixed liquor, in ultrasonic power 1-100W/cm2, supersonic frequency 20-80kHz under the conditions of 20-60 DEG C of temperature, extracts 70 minutes,
The extract solution containing qinghaosu is obtained through liquid-solid separation；
3）By step 2) obtained extract solution extracts 6 times by qinghaosu extract solution, and separation organic phase obtains qinghaosu extraction phase, raffinate
Phase-ionic liquid is recycled；
4）By step 3) obtained organic extraction mutually evaporates after recovery organic extractant to obtain qinghaosu crude product；
5）By step 4) obtained qinghaosu crude product is redissolved, and high-purity qinghaosu is further refining to obtain with column chromatography, recrystallization；
6）By step 5) after obtained ionic liquid raffinate recycles 2-8 time, addition macroporous absorbent resin stirring and adsorbing
0.5-10 hours, filter or centrifuge resin, the ionic liquid extract liquid regenerated.
Beneficial effects of the present invention：The present invention is using glyoxaline ion liquid halide salts as extractant, and water is reduction system
The diluent of viscosity, in ultrasound-enhanced lower extraction qinghaosu, using organic extractant, extracting and enriching is blue or green from qinghaosu extract solution
Artemisin, while realizing the regeneration and recycling of ionic liquid, organic extraction obtains sweet wormwood after mutually evaporating recovery organic extractant
Plain crude product, qinghaosu crude product is further refining to obtain high-purity qinghaosu, ionic liquid raffinate after being redissolved through chromatography, recrystallization
It mutually can be recycled, regenerated after being recycled for multiple times using macroreticular resin, there is the present invention extractant not fire, not wave
Send out, be lost it is small, consume energy it is low, without potential safety hazard, it is easy to operate, be easy to industrialized advantage.
Embodiment
Embodiment
A kind of technique of efficiently extracting and producing artemisinin by ionic liquid, comprises the following steps：
1) dry sweet wormwood blade of grass is carried out being crushed to powder；
2）Sweet Wormwood Herb was subjected to 90 mesh sieves, compares 2 by solid-liquid:7-2:80 add glyoxaline ion liquid halide salts and water
Mixed liquor, in ultrasonic power 1-100W/cm2, supersonic frequency 20-80kHz under the conditions of 20-60 DEG C of temperature, extracts 70 minutes,
The extract solution containing qinghaosu is obtained through liquid-solid separation；
3）By step 2) obtained extract solution extracts 6 times by qinghaosu extract solution, and separation organic phase obtains qinghaosu extraction phase, raffinate
Phase-ionic liquid is recycled；
4）By step 3) obtained organic extraction mutually evaporates after recovery organic extractant to obtain qinghaosu crude product；
5）By step 4) obtained qinghaosu crude product is redissolved, and high-purity qinghaosu is further refining to obtain with column chromatography, recrystallization；
6）By step 5) after obtained ionic liquid raffinate recycles 2-8 time, addition macroporous absorbent resin stirring and adsorbing
0.5-10 hours, filter or centrifuge resin, the ionic liquid extract liquid regenerated.
The present invention is when implementing, and the present invention is using glyoxaline ion liquid halide salts as extractant, and water is viscous for reduction system
The diluent of degree, in ultrasound-enhanced lower extraction qinghaosu, using organic extractant from qinghaosu extract solution extracting and enriching sweet wormwood
Element, while realizing the regeneration and recycling of ionic liquid, organic extraction obtains qinghaosu after mutually evaporating recovery organic extractant
Crude product, qinghaosu crude product is further refining to obtain high-purity qinghaosu, ionic liquid raffinate phase after being redissolved through chromatography, recrystallization
It can be recycled, regenerated after being recycled for multiple times using macroreticular resin, there is the present invention extractant not fire, not wave
Send out, be lost it is small, consume energy it is low, without potential safety hazard, it is easy to operate, be easy to industrialized advantage.
Claims (1)
1. a kind of technique of efficiently extracting and producing artemisinin by ionic liquid, it is characterised in that：Comprise the following steps：
1) dry sweet wormwood blade of grass is carried out being crushed to powder；
2）Sweet Wormwood Herb was subjected to 90 mesh sieves, compares 2 by solid-liquid:7-2:80 add glyoxaline ion liquid halide salts and water
Mixed liquor, in ultrasonic power 1-100W/cm2, supersonic frequency 20-80kHz under the conditions of 20-60 DEG C of temperature, extracts 70 minutes,
The extract solution containing qinghaosu is obtained through liquid-solid separation；
3）By step 2) obtained extract solution extracts 6 times by qinghaosu extract solution, and separation organic phase obtains qinghaosu extraction phase, raffinate
Phase-ionic liquid is recycled；
4）By step 3) obtained organic extraction mutually evaporates after recovery organic extractant to obtain qinghaosu crude product；
5）By step 4) obtained qinghaosu crude product is redissolved, and high-purity qinghaosu is further refining to obtain with column chromatography, recrystallization；
6）By step 5) after obtained ionic liquid raffinate recycles 2-8 time, addition macroporous absorbent resin stirring and adsorbing
0.5-10 hours, filter or centrifuge resin, the ionic liquid extract liquid regenerated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710472851.XA CN107312015A (en) | 2017-06-21 | 2017-06-21 | A kind of technique of efficiently extracting and producing artemisinin by ionic liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710472851.XA CN107312015A (en) | 2017-06-21 | 2017-06-21 | A kind of technique of efficiently extracting and producing artemisinin by ionic liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107312015A true CN107312015A (en) | 2017-11-03 |
Family
ID=60183287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710472851.XA Pending CN107312015A (en) | 2017-06-21 | 2017-06-21 | A kind of technique of efficiently extracting and producing artemisinin by ionic liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107312015A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113528488A (en) * | 2021-08-17 | 2021-10-22 | 南昌大学 | Method for preparing high-quality crude hyaluronidase product by stirring and adsorbing resin |
| CN113583017A (en) * | 2021-08-27 | 2021-11-02 | 中国科学院过程工程研究所 | Method for selectively extracting and separating artemisinin/arteannuin by using hydrophilic ionic liquid |
| CN113735874A (en) * | 2021-09-01 | 2021-12-03 | 中国科学院过程工程研究所 | Method for selectively extracting and separating artemisinin/arteannuin by hydrophobic ionic liquid |
| CN115738384A (en) * | 2022-12-13 | 2023-03-07 | 中国科学院过程工程研究所 | Ionic liquid @ SiO 2 Method for material selective separation of artemisinin/artelene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597296A (en) * | 2008-06-02 | 2009-12-09 | 中国科学院过程工程研究所 | A kind of novel method of efficiently extracting and producing artemisinin by ionic liquid |
-
2017
- 2017-06-21 CN CN201710472851.XA patent/CN107312015A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597296A (en) * | 2008-06-02 | 2009-12-09 | 中国科学院过程工程研究所 | A kind of novel method of efficiently extracting and producing artemisinin by ionic liquid |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113528488A (en) * | 2021-08-17 | 2021-10-22 | 南昌大学 | Method for preparing high-quality crude hyaluronidase product by stirring and adsorbing resin |
| CN113583017A (en) * | 2021-08-27 | 2021-11-02 | 中国科学院过程工程研究所 | Method for selectively extracting and separating artemisinin/arteannuin by using hydrophilic ionic liquid |
| CN113735874A (en) * | 2021-09-01 | 2021-12-03 | 中国科学院过程工程研究所 | Method for selectively extracting and separating artemisinin/arteannuin by hydrophobic ionic liquid |
| CN113735874B (en) * | 2021-09-01 | 2023-02-21 | 中国科学院过程工程研究所 | Method for selectively extracting and separating artemisinin/arteannuin by using hydrophobic ionic liquid |
| CN115738384A (en) * | 2022-12-13 | 2023-03-07 | 中国科学院过程工程研究所 | Ionic liquid @ SiO 2 Method for material selective separation of artemisinin/artelene |
| CN115738384B (en) * | 2022-12-13 | 2024-05-28 | 中国科学院过程工程研究所 | Ionic liquid @ SiO2Method for material selective separation of artemisinin/artemisinin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101597296B (en) | Novel method for efficiently extracting and producing artemisinin by ionic liquid | |
| CN107312015A (en) | A kind of technique of efficiently extracting and producing artemisinin by ionic liquid | |
| CN105061526B (en) | A kind of extracting method of high-purity Rubusoside | |
| CN104946383B (en) | A kind of supercritical CO2The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil | |
| CN101792373B (en) | Process for extracting, separating and purifying high-purity resveratrol | |
| CN103432562A (en) | Method for extracting fresh ginger polyphenol from fresh ginger | |
| WO2015168962A1 (en) | Method for extracting chlorogenic acid from eucommia leaves | |
| CN103664988A (en) | Extraction and separation method for artemisinin | |
| CN107955017A (en) | A kind of qinghaosu Ultrasonic reflux extraction method | |
| CN108976193B (en) | Method for extracting osthole | |
| CN116459286B (en) | Method for extracting moringa flavone from moringa leaves | |
| CN102875635B (en) | Method for comprehensively extracting protodioscin and dioscin from dioscorea nipponica | |
| CN103833805A (en) | Process for refining glycyrrhizinic acid in liquorice | |
| CN115043889B (en) | Method for extracting synephrine, hesperidin and naringin from seville orange flower | |
| CN103432205A (en) | Novel method for extracting high-purity lotus leaf flavone | |
| CN105131005A (en) | Preparation method for high content macleaya cordata alkaloid | |
| CN105524036A (en) | High-efficiency low-consumption grape seed procyanidine extraction method | |
| CN104974202B (en) | A kind of method of the extraction separation Vitexin xyloside from natural products | |
| CN116554246A (en) | Method for separating and purifying salidroside from rhodiola rosea | |
| CN115925769A (en) | Method for extracting baicalin from scutellaria baicalensis | |
| CN107235988A (en) | A kind of extracting method of qinghaosu and Artemisitene | |
| CN107857771A (en) | A kind of extraction and separation process of qinghaosu | |
| CN108299459B (en) | Method for extracting artemisinin by using polyethylene glycol solvent | |
| CN103058858A (en) | Method for extracting high-purity carnosic acid from rosemary | |
| CN107298688A (en) | A kind of purification process for extracting concentration qinghaosu |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171103 |
|
| RJ01 | Rejection of invention patent application after publication |