CN107746407A - A kind of method of sweet wormwood alkene in reduction qinghaosu - Google Patents
A kind of method of sweet wormwood alkene in reduction qinghaosu Download PDFInfo
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- CN107746407A CN107746407A CN201711142224.6A CN201711142224A CN107746407A CN 107746407 A CN107746407 A CN 107746407A CN 201711142224 A CN201711142224 A CN 201711142224A CN 107746407 A CN107746407 A CN 107746407A
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- sweet wormwood
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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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Abstract
The present invention relates to sweet wormwood production technical field, and in particular to a kind of method for reducing sweet wormwood alkene in qinghaosu.The inventive method comprises the following steps：S1. sweet wormwood petroleum ether extract is prepared, adjusts solid-liquid ratio and temperature to 25 40 DEG C；S2. take silica gel to fill post, control silica gel amount of fill, loading volume and loading flow velocity in every silica gel, complete the absorption of sample loading；S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid；S4. qinghaosu crystallization and recrystallization.A kind of method for reducing sweet wormwood alkene in qinghaosu is provided, the inventive method is suitable for lab scale, pilot scale, and especially suitable for the removal of sweet wormwood alkene in sweet wormwood extract in big production, technique is controllable, and the content by sweet wormwood alkene in qinghaosu of efficiency is less than 2%.
Description
【Technical field】
The present invention relates to sweet wormwood production technical field, and in particular to a kind of method for reducing sweet wormwood alkene in qinghaosu.
【Background technology】
Qinghaosu is that to be extracted from compound inflorescence plant Artemisia annua cauline leaf have the sesquiterpene lactone medicine of peroxy-radical, by
Chinese pharmacy man slaughter cry of a deer found that there is the characteristics of less toxic, efficient, quick-acting in 1971.Qinghaosu is after pyrimethamine, chlorine
Maximally effective antimalarial specific drug after quinoline, primary quinoline, especially for encephalic malaria and anti-chlorine quinoline malaria, have quick-acting and less toxic
Feature, it is " the only effective malaria treatment medicine in the world " to be once referred to as by the World Health Organization.The anti-malarial mechanism of action is main
The process being in treatment malaria is activated by qinghaosu produces free radical, free radical and malaria original protein binding, acts on malaria original
The film structure of worm, its vacuolar membrane, nuclear membrane and plasma membrane is set to be destroyed, mitochondrial swelling, interior outer membrane comes off, so as to former to malaria
The eucaryotic cell structure and its function of worm damage.
According to the statistics of World Health Organization, from 2000, the population of Sub-Saharan Africa area about 2.4 hundred million was benefited from
Qinghaosu conjoint therapy, about 1,500,000 people are dead caused by the therapy avoids malaria.Therefore, many African common people address respectfully it
For " east god's medicine ".In addition artemisinine also shows that tempting prospect in the treatment of other diseases.Such as anti-schistosome, regulation or
Suppress the immunologic function of body fluid, improve the conversion ratio of lymphocyte, cholagogic, eliminating the phlegm, antibechic, relieving asthma.
Current anti-malarial qinghaosu related preparations in the world, the overwhelming majority is injection.Because injection is directly injected into
In human body or in blood, if the impurity content exceeding index in medicine, allergy or other lesions are easily caused to even result in death, institute
To continue to increase with China the limitation to relative substance in injection in the world at present, in intermediate the requirement of impurity also constantly carry
Height, impurity requirement is also improved constantly in other drugs.Sweet wormwood alkene is listed in impurity in qinghaosu extract solution intermediate, because
This in qinghaosu extraction process control sweet wormwood alkene amount, be qinghaosu extractive technique the most important thing.
Sweet wormwood alkene, Artemisitene, molecular formula C15H20O5, with the molecular formula and chemical structural formula of qinghaosu all very
It is close, large-scale production process is particularly during extraction purification and is difficult to remove, turns into the problem of sweet wormwood extraction, at present on how to go
Except the research of sweet wormwood alkene in Artemisinin is also in blank stage.Sweet wormwood alkene is shown as with high performance liquid chromatography detection process
In, a miscellaneous peak before qinghaosu, based on sweet wormwood alkene, it can be brought for the qinghaosu for being mainly used as injection serious
Adverse reaction.Sweet wormwood alkene and qinghaosu it can not such as separate well, then the purity of qinghaosu will be reduced, bring serious peace
Full hidden danger.The content of sweet wormwood alkene in existing commercially available at present or outlet qinghaosu product, using area normalization method, sweet wormwood alkene contains
Measure between 2.5-3.5%.
【The content of the invention】
The goal of the invention of the present invention is：The problem of in background technology, there is provided one kind reduces sweet wormwood alkene in qinghaosu
Method, the inventive method is suitable for lab scale, pilot scale, is gone especially suitable for sweet wormwood alkene in sweet wormwood extract in big production
Remove, technique is controllable, and the content by sweet wormwood alkene in qinghaosu of efficiency is less than 2%.
To achieve these goals, the technical solution adopted by the present invention is as follows：
The method of sweet wormwood alkene, comprises the following steps in a kind of reduction qinghaosu：
S1. sweet wormwood petroleum ether extract is taken, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 1：5-20kg/L, it is quiet
Put, it is standby when the temperature of liquid to be extracted is down to 25-40 DEG C；
S2. silica gel dress post is taken to obtain silica gel splitter, the amount of fill of silica gel is 200-800kg in every silica gel splitter, so
The extract solution in step S1 is added on silica gel splitter afterwards and carried out, the sample-loading amount of the every silicagel column is 8000-
28000L extract solution, adjustable column subflow speed is 500-3500L/h, completes sample loading；
S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid, obtain sweet wormwood
Eluent, it is standby；
S4. sweet wormwood eluent is taken, condensing crystallizing dries to obtain crude product, adds alcohol toward crude product, is filtered respectively with diatomite and micropore
Film filters successively, stands still for crystals, and takes crystalline solid to produce qinghaosu.
Optimization, qinghaosu is further recrystallized, and method and crystallization are same in the recrystallization.
Optimization, calculated using area normalization method, the content of sweet wormwood alkene is less than 2% in qinghaosu.
Further optimize, the preparation method of the sweet wormwood petroleum ether extract is following any：
A. Artemisia annua is taken, is directly extracted with petroleum ether, obtains petroleum ether extract, solid-liquid ratio is adjusted, produces；
B. Artemisia annua is taken by solvent extraction, after recycling design, with petroleum ether dissolution, is adjusted solid-liquid ratio, is produced.
Further optimize, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 10-15kg/L.
Further optimize again, the sample-loading amount of the every silicagel column is 12000-25000L extract solution.
Further optimize again, the flow velocity is 1500-2500L/h.
Further optimize again, the volume ratio of the eluent petrochina ether and ethyl acetate is 90-99：1-10.
Further optimize again, the dosage of the eluent is 5-10 times of column volume.
Further optimize again, the aperture of the miillpore filter is 0.22-0.45 microns.
Further optimize again, ethanol is added into crude product and is crystallized, the mass fraction of the ethanol is 80-
95%, the dosage of the ethanol is 5-15 times of crude product.
Further optimize, when collecting median elution liquid, by detecting artemislnin content, before eluent and below
Eluent is collected separately because the high artemislnin content of impurity is low or not collected.
Further optimize, the number crystallized in step S4 is 1-4 times, and the 1st time method for crystallising is：Add in into crude product
Enter alcohol, ethanol solution is filtered successively with diatomite and miillpore filter, stand, obtain crystal I and filtrate I；Take filtrate I after
Continuous concentration, stands still for crystals, and obtains crystal II and filtrate II, merges crystal and is recrystallized as stated above.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1. present invention firstly provides being studied for how to remove sweet wormwood alkene in qinghaosu, by molten to extract solution
Agent, temperature, pillar filling species, dosage etc. are screened, and have obtained being suitable for through agent, efficient purification process；By tradition
The content of sweet wormwood alkene is substantially 3% or so in the qinghaosu that method purification process obtains, and the sweet wormwood of the inventive method after purification
Alkene content is less than 2%, can most preferably reach 0.93% in embodiment, more up to lower in actual production process, even below
0.5%.Sweet wormwood alkene is because chemical constitution and property and qinghaosu are very close, in lab scale process into large-scale production process, due to
The change of extraction purification amount is obtained with adjusting to optimum state, the present invention by constantly studying, it is necessary to tested many times
Purification process, be very suitable for removing sweet wormwood olefinic impurity content in qinghaosu in big production, save solvent, improve income.
2. ground in the present invention for the sample concentration of sample, loading volume, loading speed etc. in qinghaosu purifying
Study carefully, research in production is found, in silicagel column silica gel dosage number directly determine the size for separating sample, in production if
When silica gel dosage is less than 200kg in single post, the sample size of separation is few, material and time cost steeply rise increase by 30% with
On；And after loading is more than 800kg, column volume becomes big, even if expanding column diameter or increase length, during will also result in loading
Absorption is uneven, and pressure is excessive, has more than 15% to be in unadsorbed state in silica gel, separating effect is bad, and sweet wormwood alkene is miscellaneous from that need to make
Matter increases above more than 2.5%.
3. the present invention is dissolved the sample of loading with petroleum ether according to produce reality, regulation petroleum ether extract with
The solid-liquid ratio of sweet wormwood crude drug is 1：5-20kg/L, most preferably 10-15kg/L；What is so coordinated often want, and the applied sample amount of silica gel is
8000-28000L extract solution, pillar flow velocity are 500-3500L/h, while arrival efficiently separates, have taken into account solvent use again
Amount, production time, device requirement, it can be adapted to produce needs greatly.Because petroleum ether has very strong volatility, thus it is right before loading
Its temperature also has strict limitation, controls at 25-40 DEG C, reduces volatilization, reduces volumetric errors.
【Brief description of the drawings】
The efficient liquid phase figure of Fig. 1 test specimens 5；
The efficient liquid phase figure of Fig. 2 comparative samples 1；
In accompanying drawing, 1- solvent peaks, 2- sweet wormwood alkene, 3- qinghaosus.
【Embodiment】
With reference to embodiment, the invention will be further described.
Embodiment 1
1. a kind of method for reducing sweet wormwood alkene in qinghaosu, comprises the following steps：
S1. sweet wormwood petroleum ether extract is taken, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 1：20kg/L, stand,
It is standby when the temperature of liquid to be extracted is down to 40 DEG C；
Wherein, the preparation method of sweet wormwood petroleum ether extract is：Artemisia annua is taken by solvent extraction, after recycling design, is used
Petroleum ether dissolution, solid-liquid ratio is adjusted, is produced.
S2. silica gel dress post is taken to obtain silica gel splitter, the amount of fill of silica gel be 200kg in every silica gel splitter, then general
Extract solution in step S1 is added on silica gel splitter and carried out, and the sample-loading amount of the every silicagel column is 8000L extract solution,
Adjustable column subflow speed is 500L/h, completes sample loading；
S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid, obtain sweet wormwood
Eluent, it is standby；Wherein, the volume ratio of eluent petrochina ether and ethyl acetate is 90：10；The dosage of eluent is 10 times of posts
Volume.
S4. sweet wormwood eluent is taken, condensing crystallizing dries to obtain crude product, and alcohol is added into crude product, respectively with diatomite and micropore
Filter membrane filters successively, stands still for crystals, and takes crystalline solid to produce qinghaosu；Wherein calculated using area normalization method, it is blue or green in qinghaosu
The content of wormwood artemisia alkene is less than 2%.
Wherein, the aperture of miillpore filter is 0.22 micron.
The specific method of crystallization is：Add ethanol into crude product to be crystallized, the mass fraction of the ethanol is 80%, institute
The dosage for stating ethanol is 15 times of crude product.
Embodiment 2
1. a kind of method for reducing sweet wormwood alkene in qinghaosu, comprises the following steps：
S1. sweet wormwood petroleum ether extract is taken, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 5kg/L, stands, waits to carry
It is standby when taking the temperature of liquid to be down to 25 DEG C；
Wherein, the preparation method of sweet wormwood petroleum ether extract is：Artemisia annua is taken, is directly extracted with petroleum ether, is obtained
To petroleum ether extract, solid-liquid ratio is adjusted, is produced；
S2. silica gel dress post is taken to obtain silica gel splitter, the amount of fill of silica gel be 800kg in every silica gel splitter, then general
Extract solution in step S1 is added on silica gel splitter and carried out, and the sample-loading amount of the every silicagel column is 28000L extraction
Liquid, adjustable column subflow speed is 3500L/h, completes sample loading；
S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid, obtain sweet wormwood
Eluent, it is standby；Wherein, the volume ratio of eluent petrochina ether and ethyl acetate is 97.1：2.9；The dosage of eluent is 5 times
Column volume.
S4. sweet wormwood eluent is taken, condensing crystallizing dries to obtain crude product, and alcohol is added into crude product, respectively with diatomite and micropore
Filter membrane filters successively, stands still for crystals, and takes crystalline solid to produce qinghaosu；Wherein calculated using area normalization method, it is blue or green in qinghaosu
The content of wormwood artemisia alkene is less than 2%.
Wherein, the aperture of miillpore filter is 0.45 micron.
The specific method of crystallization is：Add ethanol into crude product to be crystallized, the mass fraction of the ethanol is 95%, institute
The dosage for stating ethanol is 5 times of crude product.
Embodiment 3
1. a kind of method for reducing sweet wormwood alkene in qinghaosu, comprises the following steps：
S1. sweet wormwood petroleum ether extract is taken, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 1：10kg/L, stand,
It is standby when the temperature of liquid to be extracted is down to 30 DEG C；
Wherein, the preparation method of sweet wormwood petroleum ether extract is：Artemisia annua is taken, is directly extracted with petroleum ether, is obtained
To petroleum ether extract, solid-liquid ratio is adjusted, is produced；
S2. silica gel dress post is taken to obtain silica gel splitter, the amount of fill of silica gel be 350kg in every silica gel splitter, then general
Extract solution in step S1 is added on silica gel splitter and carried out, and the sample-loading amount of the every silicagel column is 12000L extraction
Liquid, adjustable column subflow speed is 1500L/h, completes sample loading；
S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid, obtain sweet wormwood
Eluent, it is standby；Wherein, the volume ratio of eluent petrochina ether and ethyl acetate is 96：4；The dosage of eluent is 6 times of cylinders
Product；
S4. sweet wormwood eluent is taken, condensing crystallizing dries to obtain crude product, and alcohol is added into crude product, respectively with diatomite and micropore
Filter membrane filters successively, stands still for crystals, and takes crystalline solid to produce qinghaosu；Wherein calculated using area normalization method, it is blue or green in qinghaosu
The content of wormwood artemisia alkene is less than 2%.
Wherein, the aperture of miillpore filter is 0.22 micron.
The specific method of crystallization is：Add ethanol into crude product to be crystallized, the mass fraction of the ethanol is 85%, institute
The dosage for stating ethanol is 12.5 times of crude product.
Embodiment 4
1. a kind of method for reducing sweet wormwood alkene in qinghaosu, comprises the following steps：
S1. sweet wormwood petroleum ether extract is taken, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 15kg/L, stands, treats
It is standby when the temperature of extract solution is down to 35 DEG C；
Wherein, the preparation method of sweet wormwood petroleum ether extract is following any：Artemisia annua is taken by solvent extraction, recovery
After solvent, with petroleum ether dissolution, solid-liquid ratio is adjusted, is produced.
S2. silica gel dress post is taken to obtain silica gel splitter, the amount of fill of silica gel be 650kg in every silica gel splitter, then general
Extract solution in step S1 is added on silica gel splitter and carried out, and the sample-loading amount of the every silicagel column is 25000L extraction
Liquid, adjustable column subflow speed is 2500L/h, completes sample loading；
S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid, obtain sweet wormwood
Eluent, it is standby；Wherein, the volume ratio of eluent petrochina ether and ethyl acetate is 99：1；The dosage of eluent is 7.5 times of posts
Volume.
S4. sweet wormwood eluent is taken, condensing crystallizing dries to obtain crude product, and alcohol is added into crude product, respectively with diatomite and micropore
Filter membrane filters successively, stands still for crystals, and takes crystalline solid to produce qinghaosu；Wherein calculated using area normalization method, it is blue or green in qinghaosu
The content of wormwood artemisia alkene is less than 2%.
Wherein, the aperture of miillpore filter is 0.45 micron.
The specific method of crystallization is：Add ethanol into crude product to be crystallized, the mass fraction of the ethanol is 90%, institute
The dosage for stating ethanol is 7 times of crude product.
Embodiment 5
1. a kind of method for reducing sweet wormwood alkene in qinghaosu, comprises the following steps：
S1. sweet wormwood petroleum ether extract is taken, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 1：18kg/L, stand,
It is standby when the temperature of liquid to be extracted is down to 29 DEG C；
Wherein, the preparation method of sweet wormwood petroleum ether extract is following any：Artemisia annua is taken, is directly entered with petroleum ether
Row extraction, obtains petroleum ether extract, adjusts solid-liquid ratio, produces；
S2. silica gel dress post is taken to obtain silica gel splitter, the amount of fill of silica gel be 450kg in every silica gel splitter, then general
Extract solution in step S1 is added on silica gel splitter and carried out, and the sample-loading amount of the every silicagel column is 2100L extract solution,
Adjustable column subflow speed is 2200L/h, completes sample loading；
S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid, obtain sweet wormwood
Eluent, it is standby；Wherein, the volume ratio of eluent petrochina ether and ethyl acetate is 97.5：2.5；The dosage of eluent is 7.5
Times column volume.
S4. sweet wormwood eluent is taken, condensing crystallizing dries to obtain crude product, and alcohol is added into crude product, respectively with diatomite and micropore
Filter membrane filters successively, stands still for crystals, and takes crystalline solid to produce qinghaosu；Wherein calculated using area normalization method, it is blue or green in qinghaosu
The content of wormwood artemisia alkene is less than 2%.
Wherein, the aperture of miillpore filter is 0.22 micron.
The specific method of crystallization is：Add ethanol into crude product to be crystallized, the mass fraction of the ethanol is 93%, institute
The dosage for stating ethanol is 9 times of crude product.
Embodiment 6 contrasts implementation result
Using high-efficient liquid phase technique each sample is detected, calculating sweet wormwood alkene in qinghaosu according to area normalization method contains
Amount.
1. sample preparation：Sample 50mg or so is taken, it is accurately weighed, put in 10ml measuring bottles, add flowing phased soln and be diluted to
Scale, shake up, 0.45 μm of membrane filtration.
2. test sample：The qinghaosu sample for taking the method by embodiment 1-5 to be prepared is test specimen 1-5.In pressing
State's Authorization Notice No. is the artemisinin-like that the method for embodiment 1 in CN102219790B Green extraction process for artemisinin methods obtains
Product are control sample 1；Being prepared as described in Example 5, change eluent into petroleum ether, other method is same with embodiment 5,
Obtain control sample 2；
3. sample detection condition：
Chromatographic column：The strong silica gel that closes of octadecylsilane is filler；
Column temperature：30℃；
Wavelength：216nm；
Mobile phase：Acetonitrile：Water=50：50；
Flow velocity：1.0ml/min；
Sampling volume：20μl；
Run time：25min
4. the confirmation of composition in collection of illustrative plates：Using qinghaosu and sweet wormwood alkene standard sample, dissolved with methanol, in same inspection
Under the conditions of survey, confirmed according to appearance time.
5. computational methods：Sweet wormwood alkene is calculated using area normalization method to impurity sweet wormwood alkene (being called impurity A in the present invention)
Content.
The content statistics of sweet wormwood alkene in each sample of table 1
| Sweet wormwood alkene retention time | Sweet wormwood alkene content % | |
| Test specimen 1 | 11.462 | 1.96 |
| Test specimen 2 | 11.471 | 1.21 |
| Test specimen 3 | 11.468 | 1.78 |
| Test specimen 4 | 11.459 | 1.19 |
| Test specimen 5 | 11.476 | 0.93% |
| Control sample 1 | 11.451 | 2.80% |
| Control sample 2 | 11.460 | 2.76% |
From table, it can be seen that the content of sweet wormwood alkene is respectively less than 2% in 1-5 of the embodiment of the present invention, and is entered with conventional method
Row extraction, the content for the refined rear sweet wormwood alkene of control sample for crossing post are still up to 3%, such as the green grass or young crops in control sample in this experiment
Wormwood artemisia alkene content is above 2.6%, and 2.5% can be also higher than in the case of.Test specimen 5 and the efficient liquid phase pair for compareing product in the same old way
See accompanying drawing 1 than figure.
Described above is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, the equal change completed or modification change under the technical spirit suggested by all present invention, all should belong to
Cover the scope of the claims in the present invention.
Claims (10)
- A kind of 1. method for reducing sweet wormwood alkene in qinghaosu, it is characterised in that comprise the following steps：S1. sweet wormwood petroleum ether extract is taken, the solid-liquid ratio of the extract solution and sweet wormwood crude drug is 1：5-20kg/L, stand, treat It is standby when the temperature of extract solution is down to 25-40 DEG C；S2. silica gel dress post is taken to obtain silica gel splitter, the amount of fill of silica gel be 200-800kg in every silica gel splitter, then general Extract solution in step S1 is added on silica gel splitter and carried out, and the sample-loading amount of the every silicagel column is 8000-28000L's Extract solution, adjustable column subflow speed is 500-3500L/h, completes sample loading；S3. take the mixed liquor of petroleum ether and ethyl acetate to be eluted as eluent, collect median elution liquid, obtain sweet wormwood elution Liquid, it is standby；S4. take sweet wormwood eluent, condensing crystallizing dries to obtain crude product, and alcohol is added toward crude product, respectively with diatomite and miillpore filter according to Secondary filtering, stands still for crystals, and takes crystalline solid to produce qinghaosu.
- 2. a kind of method for reducing sweet wormwood alkene in qinghaosu according to claim 1, it is characterised in that using area normalization Change method calculates, and the content of sweet wormwood alkene is less than 2% in qinghaosu.
- A kind of 3. method for reducing sweet wormwood alkene in qinghaosu according to claim 1, it is characterised in that the sweet wormwood oil The preparation method of ether extract solution is following any：A. Artemisia annua is taken, is directly extracted with petroleum ether, obtains petroleum ether extract, solid-liquid ratio is adjusted, produces；B. Artemisia annua is taken by solvent extraction, after recycling design, with petroleum ether dissolution, is adjusted solid-liquid ratio, is produced.
- 4. it is according to claim 1 it is a kind of reduce qinghaosu in sweet wormwood alkene method, it is characterised in that the extract solution with The solid-liquid ratio of sweet wormwood crude drug is 10-15kg/L.
- A kind of 5. method for reducing sweet wormwood alkene in qinghaosu according to claim 1, it is characterised in that the every silica gel The sample-loading amount of post is 12000-25000L extract solution.
- 6. a kind of method for reducing sweet wormwood alkene in qinghaosu according to claim 1, it is characterised in that the flow velocity is 1500-2500L/h。
- 7. a kind of method for reducing sweet wormwood alkene in qinghaosu according to claim 1, it is characterised in that in the eluent The volume ratio of petroleum ether and ethyl acetate is 90-99：1-10.
- 8. a kind of method for reducing sweet wormwood alkene in qinghaosu according to claim 7, it is characterised in that the eluent Dosage is 5-10 times of column volume.
- 9. the method for sweet wormwood alkene in a kind of reduction qinghaosu according to claim 1 or 8, it is characterised in that the micropore The aperture of filter membrane is 0.22-0.45 microns.
- 10. a kind of method for reducing sweet wormwood alkene in qinghaosu according to claim 1, it is characterised in that add into crude product Enter ethanol to be crystallized, the mass fraction of the ethanol is 80-95%, and the dosage of the ethanol is 5-15 times of crude product.
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Cited By (4)
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| CN109651391A (en) * | 2018-12-27 | 2019-04-19 | 广西仙草堂制药有限责任公司 | A method of qinghaosu is recycled from qinghaosu recrystallization waste material |
| CN111141846A (en) * | 2019-12-31 | 2020-05-12 | 广西仙草堂制药有限责任公司 | Method for measuring content of artemisinin in sweet wormwood herb |
| 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 |
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| 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 |
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