CN107793430A - A kind of method of purification of qinghaosu - Google Patents
A kind of method of purification of qinghaosu Download PDFInfo
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- CN107793430A CN107793430A CN201711415239.5A CN201711415239A CN107793430A CN 107793430 A CN107793430 A CN 107793430A CN 201711415239 A CN201711415239 A CN 201711415239A CN 107793430 A CN107793430 A CN 107793430A
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- qinghaosu
- silica gel
- post
- miscellaneous
- mixing
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a kind of method of purification of qinghaosu, comprise the following steps：1）Liquid processed, it is first that sweet wormwood grass meal is broken, then add 13 times（L/㎏）No. 6 solvent naphthas, refluxing extraction 6 hours at a temperature of 56 DEG C；2）Batch mixing, the heat fusing cream below 65 DEG C；The medicinal extract after hot melt, medicinal extract mixing silica gel are weighed by 110 ㎏/post；3）Post is filled, to utilize No. 6 solvent naphthas with ethyl acetate with 65:The solvent of 7 mixing does eluent, wet method dress post, obtains silicagel column；4）Stand, with No. 6 solvent naphthas and ethyl acetate with 65:The solvents of 7 mixing do eluent, rush post without qinghaosu, containing miscellaneous qinghaosu and without miscellaneous qinghaosu, respectively to being eluted without qinghaosu, containing miscellaneous qinghaosu and without miscellaneous qinghaosu；5）Eluent is collected, concentration, places 24 hours and crystallizes, centrifugation, obtain qinghaosu crude product；6）It is refined, obtained qinghaosu crude product is further refined, the present invention has the advantages of preparation technology is simple, purification efficiency is higher, preparation cost is relatively low in a word.
Description
Technical field
The invention belongs to qinghaosu preparation technology field, and in particular to a kind of method of purification of qinghaosu.
Background technology
Qinghaosu is a kind of colourless acicular crystal for extracting to obtain from compound inflorescence plant Artemisia annua i.e. Chinese medicine artemisia leaf,
Drug containing sweet wormwood, qinghaosu are not the maximally effective antimalarial specific drugs after pyrimethamine, chloroquine, primary quinoline in its stem, especially
For encephalic malaria and anti-chlorine quinoline malaria, there is the characteristics of quick-acting and less toxic, be once referred to as " in the world only by the World Health Organization
One effective malaria treatment medicine "；The anti-malarial mechanism of action essentially consists in passes through qinghaosu activation production in the process for treating malaria
Raw free radical, free radical and malaria original protein binding, 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 as to be damaged to the eucaryotic cell structure and its function of plasmodium；In addition it is blue or green
Punt-pole element also shows that tempting prospect in the treatment of other diseases；As anti-schistosome, regulation or suppress body fluid immunologic function,
The conversion ratio of lymphocyte is improved, cholagogic, eliminating the phlegm, antibechic, is relievingd asthma, therefore qinghaosu has great medical market prospect；
But qinghaosu its purity obtained by current methods is used often not reach requirement, it is necessary to further be carried to qinghaosu
Pure, when carrying out purification operation, existing operation will often expend substantial amounts of raw material, and the flow of its operation is also more numerous
It is trivial, it is impossible to meet the needs of large-scale production, it is therefore necessary to which the method for purification of qinghaosu is improved.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, and provide a kind of method of purification of qinghaosu.
The object of the present invention is achieved like this：A kind of method of purification of qinghaosu, comprises the following steps：
1）Liquid processed, it is first that sweet wormwood grass meal is broken, then add 13 times（L/㎏）No. 6 solvent naphthas, refluxing extraction 6 is small at a temperature of 56 DEG C
When, extract solution concentration, receive cream and obtain qinghaosu medicinal extract；
2）Batch mixing, the heat fusing cream below 65 DEG C；The medicinal extract after hot melt is weighed by 110 ㎏/post, medicinal extract mixing silica gel, drying, is obtained
Spice silica gel；Silica gel amount=medicinal extract the amount × Silica gel activated, the Silica gel activated silica gel amount for needed for often suction 1ml water；
3）Post is filled, to utilize No. 6 solvent naphthas with ethyl acetate with 65:The solvent of 7 mixing does eluent, wet method dress post, obtains silica gel
Post；
4）Stand, with No. 6 solvent naphthas and ethyl acetate with 65:The solvent of 7 mixing does eluent, rushes post and obtains without qinghaosu, containing miscellaneous
Qinghaosu and without miscellaneous qinghaosu, respectively to being eluted without qinghaosu, containing miscellaneous qinghaosu and without miscellaneous qinghaosu；
5）Eluent is collected, concentration, places 24 hours and crystallizes, centrifugation, obtain qinghaosu crude product；
6）It is refined, obtained qinghaosu crude product is further refined.
Beneficial effects of the present invention：The qinghaosu method for extraction and purification of the present invention, containing miscellaneous qinghaosu, the richness without miscellaneous qinghaosu
Collection degree is high, and the purity without miscellaneous qinghaosu crude product is up to more than 95%, up to more than 98% after refining；It is smart from sweet wormwood grass to qinghaosu
The whole recovery rate of product is up to more than 75% 2）The qinghaosu method for extraction and purification of the present invention, from sweet wormwood grass to qinghaosu fine work
Whole recovery rate is up to more than 75%；Follow-up process for refining is simple；Silica gel dosage is small, and activation method is simple, in a word present invention tool
There is the advantages of preparation technology is simple, purification efficiency is higher, preparation cost is relatively low.
Embodiment
Embodiment
A kind of method of purification of qinghaosu, comprises the following steps：
1）Liquid processed, it is first that sweet wormwood grass meal is broken, then add 13 times（L/㎏）No. 6 solvent naphthas, refluxing extraction 6 is small at a temperature of 56 DEG C
When, extract solution concentration, receive cream and obtain qinghaosu medicinal extract；
2）Batch mixing, the heat fusing cream below 65 DEG C；The medicinal extract after hot melt is weighed by 110 ㎏/post, medicinal extract mixing silica gel, drying, is obtained
Spice silica gel；Silica gel amount=medicinal extract the amount × Silica gel activated, the Silica gel activated silica gel amount for needed for often suction 1ml water；
3）Post is filled, to utilize No. 6 solvent naphthas with ethyl acetate with 65:The solvent of 7 mixing does eluent, wet method dress post, obtains silica gel
Post；
4）Stand, with No. 6 solvent naphthas and ethyl acetate with 65：The solvent of 7 mixing does eluent, rushes post and obtains without qinghaosu, containing miscellaneous
Qinghaosu and without miscellaneous qinghaosu, respectively to being eluted without qinghaosu, containing miscellaneous qinghaosu and without miscellaneous qinghaosu；
5）Eluent is collected, concentration, places 24 hours and crystallizes, centrifugation, obtain qinghaosu crude product；
6）It is refined, obtained qinghaosu crude product is further refined.
The present invention takes the silica gel column chromatography method of " wet method dress post, dry method loading " when implementing.Wet method dress post, be by
Silica gel and appropriate solvent（It is general to use eluent）After mixing thoroughly, the dress column method of pillar is reloaded into.Dry method loading, it is that will treat point
From medicinal extract mixed thoroughly with silica gel, dry after spice silica gel is added to pillar upper strata again.Inventor sends out breakthroughly through numerous studies
It is existing, in the silica gel column chromatography method of " wet method dress post, dry method loading ", filled by the silica gel amount strictly screened for spice with being used for
The silica gel amount of post, and control for the ratio between the silica gel of spice and the silica gel amount for filling post, not only without green grass or young crops in eluent
Artemisin, containing miscellaneous qinghaosu, can be with completely separable without miscellaneous qinghaosu, and enrichment degree containing miscellaneous qinghaosu, without miscellaneous qinghaosu is high,
To it is follow-up it is refined bring conveniently, the present invention has that preparation technology is simple, purification efficiency is higher, it is lower-cost to prepare in a word
Advantage.
Claims (1)
- A kind of 1. method of purification of qinghaosu, it is characterised in that：Comprise the following steps：1）Liquid processed, it is first that sweet wormwood grass meal is broken, then add 13 times（L/㎏）No. 6 solvent naphthas, refluxing extraction 6 is small at a temperature of 56 DEG C When, extract solution concentration, receive cream and obtain qinghaosu medicinal extract；2）Batch mixing, the heat fusing cream below 65 DEG C；The medicinal extract after hot melt is weighed by 110 ㎏/post, medicinal extract mixing silica gel, drying, is obtained Spice silica gel；Silica gel amount=medicinal extract the amount × Silica gel activated, the Silica gel activated silica gel amount for needed for often suction 1ml water；3）Post is filled, to utilize No. 6 solvent naphthas with ethyl acetate with 65:The solvent of 7 mixing does eluent, wet method dress post, obtains silica gel Post；4）Stand, with No. 6 solvent naphthas and ethyl acetate with 65:The solvent of 7 mixing does eluent, rushes post and obtains without qinghaosu, containing miscellaneous Qinghaosu and without miscellaneous qinghaosu, respectively to being eluted without qinghaosu, containing miscellaneous qinghaosu and without miscellaneous qinghaosu；5）Eluent is collected, concentration, places 24 hours and crystallizes, centrifugation, obtain qinghaosu crude product；6）It is refined, obtained qinghaosu crude product is further refined.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711415239.5A CN107793430A (en) | 2017-12-25 | 2017-12-25 | A kind of method of purification of qinghaosu |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711415239.5A CN107793430A (en) | 2017-12-25 | 2017-12-25 | A kind of method of purification of qinghaosu |
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| CN107793430A true CN107793430A (en) | 2018-03-13 |
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| CN201711415239.5A Pending CN107793430A (en) | 2017-12-25 | 2017-12-25 | A kind of method of purification of qinghaosu |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110038322A (en) * | 2019-04-24 | 2019-07-23 | 上海复旦复华药业有限公司 | A kind of tripterygium glycosides chromatographic silica gel dress column method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242335A (en) * | 2013-04-28 | 2013-08-14 | 四川省裕通生物技术有限公司 | Method for extracting and purifying artemisinin |
-
2017
- 2017-12-25 CN CN201711415239.5A patent/CN107793430A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242335A (en) * | 2013-04-28 | 2013-08-14 | 四川省裕通生物技术有限公司 | Method for extracting and purifying artemisinin |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110038322A (en) * | 2019-04-24 | 2019-07-23 | 上海复旦复华药业有限公司 | A kind of tripterygium glycosides chromatographic silica gel dress column method |
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Application publication date: 20180313 |