CN110105195A - A method of extracting dihydroartemisinic acid from sweet wormwood wax oil - Google Patents
A method of extracting dihydroartemisinic acid from sweet wormwood wax oil Download PDFInfo
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- CN110105195A CN110105195A CN201910279381.4A CN201910279381A CN110105195A CN 110105195 A CN110105195 A CN 110105195A CN 201910279381 A CN201910279381 A CN 201910279381A CN 110105195 A CN110105195 A CN 110105195A
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Abstract
A method of extracting dihydroartemisinic acid from qinghaosu wax oil, comprising the following steps: (1) extract filtering: (2) cross chromatographic column: acid is adjusted in (3) abstraction impurity removal (4) concentration: (5) extraction concentration: (6) crystallization filters: (7) crude product refining.Present invention separation and Extraction from the by-product sweet wormwood wax oil of qinghaosu production process removes terpene substances similar with dihydroartemisinic acid structure but not being saponified removing by chromatography, is then concentrated, extracts, being purified into the dihydroartemisinic acid of high-quality, purity >=99%；In addition, the present invention turns waste into wealth, the transformation efficiency that sweet wormwood prepares qinghaosu is improved, saves artemisia annua raw material resources, reduces organic solvent usage amount, pollution of the qinghaosu production process waste to environment is reduced, to promote the comprehensive exploitation and utilization of Artemisia annua.
Description
Technical field
The present invention relates to a kind of methods for extracting dihydroartemisinic acid, and in particular to one kind extracts dihydro from qinghaosu wax oil
The method of Arteannuic acid.
Background technique
Qinghaosu (Arteannuin) is that the one kind extracted from Chinese medicine artemisia annua (Artemisa annua) contains peroxide
Bridge sesquiterpene lactone is efficient, less toxic antimalarial agent.Although qinghaosu has multi-drug resistant plasmodium very much
Effect, but the plantation sweet wormwood period is long, extraction process is complicated, limits throughput, and supply is insufficient, and most malaria patients hold market of daring not accept
Price.And except containing in addition to qinghaosu, also containing other sesquiterpenoids ingredients in artemisia annua, as qinghaosu G, Qinghaosu I, Qinghaosu II,
Qinghaosu III, sweet wormwood D prime, penta element of sweet wormwood, table deoxidation Qinghaosu II, artemisinol, methyl arteannuate, Arteannuic acid, 6,7- dehydrogenation
Arteannuic acid, dihydroartemisinic acid etc..Wherein the utility value of Arteannuic acid and dihydroartemisinic acid content is maximum.Dihydroartemisinic acid is sweet wormwood
The semi-synthetic intermediate product of element, is the advanced stage precursor of antimalarial compound qinghaosu.Specific synthesis process are as follows: Arteannuic acid → dihydro is green
Artemisic acid → dioxy sweet wormwood acid peroxide → qinghaosu.
The production of existing qinghaosu uses column chromatography substantially, in process of production, to extract based on qinghaosu, but in column layer
Analysis elution and crystallization when, by-product dihydroartemisinic acid is also extracted mixed with a large amount of wax oil after be treated as at waste
Reason, qinghaosu price 1100~1500 yuan/kg of ability currently on the market, precursor substance of double hydrogen Arteannuic acids as qinghaosu, no
The waste that a large amount of organic solvents cause resource is only consumed, the yield of qinghaosu is also reduced, is unfavorable for the sustainable development of industry.
103694106 A of CN discloses a kind of method of extraction purification dihydroartemisinic acid from qinghaosu wax oil, it be by
Sodium bicarbonate aqueous solution is added in wax oil, heats, after wax oil is in all molten condition, is adjusted with saturated sodium bicarbonate aqueous solution
PH value is 9~9.5, is stirred, centrifugation；Degreasing is extracted by petroleum ether and stirring is added in centrifugate；Aqueous alkali after degreasing is added
Hydrochloric acid is added after the remaining petroleum ether of heat abstraction, adjusts pH value to 5~6, lets cool to room temperature crystallization；By crystal with acetic acid second
Recrystallization can obtain dihydroartemisinic acid product after ester dissolution.
Double hydrogen Arteannuic acids are become water-soluble sodium salt using alkali by process above, are then centrifuged for insoluble impurity mistake
Filter, then carries out degreasing impurity elimination with petroleum ether.But the technique impurity elimination ability is very limited, when finally crystallization, impurity accounting meeting
Significantly more than product volume can make a large amount of product be difficult to crystallization, influence quality in this way, the higher cost of corresponding purifying purification, difficult
With marketization application.
Summary of the invention
The technical problem to be solved by the present invention is to overcome that crystallization of the existing technology is difficult, caused by crystallization not exclusively
The problems such as yield is low, purification is difficult provides a kind of effectively separate from the by-product sweet wormwood wax oil of qinghaosu production process and mentions
It takes, concentrates and purifies out the dihydroartemisinic acid of high-quality, improve the transformation efficiency that sweet wormwood prepares qinghaosu, save artemisia annua raw material
Resource reduces qinghaosu production process waste to the side for extracting dihydroartemisinic acid in the slave qinghaosu wax oil of the pollution of environment
Method.
The technical solution adopted by the present invention to solve the technical problems is as follows: it is green that one kind extracting dihydro from qinghaosu wax oil
The method of artemisic acid, comprising the following steps:
(1) it extracts filtering: sweet wormwood wax oil, methanol, water and piece alkali being added in agitator tank and is stirred, stands to solution and is layered,
It takes supernatant to be filtered, obtains wax oil extracting solution；
(2) it crosses chromatographic column: wax oil extracting solution obtained by step (1) is crossed into resin column, the efflux after collecting upper prop obtains chromatographic column receipts
Liquid collecting；
(3) concentrate abstraction impurity removal: chromatographic column collection liquid obtained by step (2) is concentrated, concentrate is obtained；Be added extractant into
Row extraction, obtains degreasing concentrate；
(4) concentrate tune acid: by the resulting degreasing concentrate of step (3), acid solution is added and adjusts pH value, obtains neutralization solution；
(5) extraction concentration: extractant is added, is extracted, obtains extract liquor, then extract liquor is concentrated under reduced pressure, must extract
Take concentrated liquor；
(6) crystallization filters: extraction concentrate obtained by step (5) being stored at room temperature crystallization, dihydroartemisinic acid crude product is obtained after suction filtration；
(7) crude product refining: the methanol of dihydroartemisinic acid crude product obtained by step (6) is dissolved completely, filtering and impurity removing is concentrated, crystallization
It filters, washes crystalline substance, it is dry,.
Further, the volumetric concentration for the methanol being added in step (1) is 50~80%(preferably 70%), dosage is sweet wormwood wax oil
18~25 times (preferably 20 times).
Further, in step (1), the dosage of the piece alkali of addition is 1/10~1/9 times (preferably 1/10 times) of sweet wormwood wax oil.
Further, agitator tank described in step (1) opens stirring before feeding intake, and starts timing after the completion of feeding intake, persistently stirs
It mixes 4~12 hours (preferably 12h).
Further, chromatographic column collection liquid obtained by step (2) is concentrated into the 1/10~1/9 of original volume, obtained by step (3)
Concentrate；It is added and is extracted relative to the extractant of 2~3 times of volumes of concentrate, extracted 50~60 minutes.
Further, in step (4), the acid solution is the hydrochloric acid solution of mass concentration 33%；PH value is adjusted to 5~7.
Further, extractant described in step (3) and step (5) be petroleum ether that boiling range is 60~90 DEG C or industry oneself
Alkane (preferably petroleum ether).
Further, in step (5), the extractant for being equivalent to and neutralizing 2~4 times of volumes of solution obtained by step (4) is added, even
Continuous extraction 2~3 times；Extract liquor is concentrated under reduced pressure into the 1/4~1/3 of original volume；Thickening temperature is controlled at 70 DEG C of <.
Further, in step (7), the volume for dissolving methanol used in dihydroartemisinic acid crude product is dihydroartemisinic acid crude product volume
2~4 times.
The method that dihydroartemisinic acid is extracted from sweet wormwood wax oil of the present invention, it is for better dissolving wax that methanol, which is added,
Oil makes wax oil scatter, so that the dihydroartemisinic acid in sweet wormwood wax oil is reacted the double hydrogen Arteannuic acids of generation by piece alkali with piece alkali
It receives salt, forms water-soluble sodium salt；Resin column, resin column adsorbing contaminant were carried out later, but double hydrogen Arteannuic acids were not adsorbed,
Further it is separated off terpene substances that are similar with dihydroartemisinic acid structure but not being saponified removing；Recycle the methanol in extracting solution
Afterwards, then with organic solvent by the extracting solution (alkalinity) after concentration extract oil-soluble impurity, later concentrate acid adding tune pH to 5~
7, so that its reaction is regenerated dihydroartemisinic acid (oil-soluble), petroleum ether or industrial hexane is added to extract double hydrogen Arteannuic acids, extraction
Liquid concentration lets cool crystallization, and crystallization filters, and obtains dihydroartemisinic acid crude product；Then dihydroartemisinic acid crude product is tied again by methanol
Crystal method purification, obtains the dihydroartemisinic acid of high-purity.
The invention has the advantages that: (1) relative to prior art, increases the step of chromatography cleans, most of due to eliminating
Impurity, dihydroartemisinic acid can be efficiently separated into extraction from the by-product sweet wormwood wax oil of qinghaosu production process, then dense
Contracting is purified into the dihydroartemisinic acid crude product of high-quality, and purity >=95% uses refining methanol one to reduce the number of purification
Secondary double hydrogen Arteannuic acid finished products that purity >=95% can be obtained；(2) be conducive to the crystallization of double hydrogen Arteannuic acids, so that crystallization is more complete,
To improve the yield of double hydrogen Arteannuic acids, that is, the transformation efficiency that sweet wormwood grass prepares qinghaosu is improved, saves artemisia annua raw material money
Organic solvent usage amount is reduced in source, and extraction process is that cold soaking extracts, and production cost can be much lower, and price can have very much on the market
Competitiveness；(3) turn waste into wealth, pollution of the qinghaosu production process waste to environment is reduced, to promote the comprehensive of Artemisia annua
It closes and develops and utilizes.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Chemical reagent used in the embodiment of the present invention is obtained by routine business approach unless otherwise specified.
Embodiment 1
The present embodiment the following steps are included:
(1) it extracts filtering: 100kg sweet wormwood wax oil, the methanol-water of 2000L70% and 10kg piece alkali being added in agitator tank and is stirred
It mixes, room temperature is extracted 4 hours, is stood to solution and is layered, takes supernatant to be filtered, obtain wax oil extracting solution, extracting solution was centrifuged
Filter, obtains clear wax oil extracting solution；Repetitive operation 4 times, 5 crowdes of extracting solution 9600L are collected altogether；
(2) it crosses chromatographic column: wax oil extracting solution obtained by step (1) is crossed into 500kgDX-7 resin column (production of Xi'an Lan Xiao resin processing plant),
Efflux after collecting upper prop, obtains chromatographic column collection liquid 10100L；
(3) concentrate abstraction impurity removal: being concentrated into 1500L for chromatographic column collection liquid obtained by step (2), be added 3000L petroleum ether or
Industrial hexane extracts 60 minutes, fat-soluble impurity is removed, petroleum ether or industrial hexane are recycled, degreasing concentrate is obtained
1500L；
(4) acid is adjusted in concentration: by degreasing concentrate obtained by step (3), 33% food grade salts acid solution of mass concentration is added, adjusts pH
Value must neutralize solution 1550L to 7；
(5) concentration is extracted: using 3000L petroleum ether to step (4) gained neutralization solution extraction 60 minutes, coextraction 2 times, then will
Dense be concentrated under reduced pressure (thickening temperature control is at 70 DEG C or less) of extract liquor are reduced to 65L volume to get extraction concentrated liquor；
(5) crystallization filters: extraction concentrated liquor obtained by step (5) being stored at room temperature crystallization, it is thick to obtain dihydroartemisinic acid after suction filtration
Product 28.9kg；
(6) crude product refining: the pure methanol of 87L of dihydroartemisinic acid crude product 28.9kg obtained by step (6) is dissolved completely, crosses and filters out
Miscellaneous, concentration, crystallization filters, and washes crystalline substance, dry, obtain dihydroartemisinic acid finished product 26.1kg.
The present embodiment conversion ratio is 5.22%, and obtained sampled detection ((HPLC)) its purity of dihydroartemisinic acid finished product is
99.2%。
Embodiment 2
The present embodiment the following steps are included:
(1) it extracts filtering: 100kg sweet wormwood wax oil, the methanol-water of 1800L70% and 10kg piece alkali being added in agitator tank and is stirred
It mixes, room temperature is extracted 4 hours, is stood to solution and is layered, takes supernatant to be filtered, obtain wax oil extracting solution, extracting solution was centrifuged
Filter, obtains clear wax oil extracting solution；Repetitive operation 4 times, 5 crowdes of extracting solution 9500L are collected altogether；
(2) it crosses chromatographic column: wax oil extracting solution obtained by step (1) is crossed into 500kgDX-7 resin column (production of Xi'an Lan Xiao resin processing plant),
Efflux after collecting upper prop, obtains chromatographic column collection liquid 9900L；
(3) concentrate abstraction impurity removal: being concentrated into 1500L for chromatographic column collection liquid obtained by step (2), be added 3000L petroleum ether or
Industrial hexane extracts 60 minutes, fat-soluble impurity is removed, petroleum ether or industrial hexane are recycled, degreasing concentrate is obtained
1500L；
(4) acid is adjusted in concentration: by chromatographic column collection liquid extracted obtained by step (3), it is molten that 33% food grade hydrochloric acid of mass concentration is added
Liquid adjusts pH value to 7, must neutralize solution 1550L；
(5) extraction concentration: neutralizing solution obtained by the step (4) using 3000L petroleum ether, extracts 60 minutes, and coextraction 2 times, then
(thickening temperature is controlled at 70 DEG C or less) is concentrated under reduced pressure in extract liquor and is concentrated into 70L volume to get extraction concentrated liquor；
(5) crystallization filters: extraction concentrated liquor obtained by step (5) being stored at room temperature crystallization, it is thick to obtain dihydroartemisinic acid after suction filtration
Product 13.8kg；
(6) crude product refining: the pure methanol of 88L of dihydroartemisinic acid crude product 29.8kg obtained by step (6) is dissolved completely, crosses and filters out
Miscellaneous, concentration, crystallization filters, and washes crystalline substance, dry, obtain 26.8 kg of dihydroartemisinic acid finished product.
The present embodiment conversion ratio is 5.36%, and obtained sampled detection (HPLC) its purity of dihydroartemisinic acid finished product is
99.5%。
Embodiment 3
The present embodiment the following steps are included:
(1) it extracts filtering: 100kg sweet wormwood wax oil, the methanol-water of 2000L70% and 10kg piece alkali being added in agitator tank and is stirred
It mixes, room temperature is extracted 12 hours, is stood to solution and is layered, takes supernatant to be filtered, obtain wax oil extracting solution, extracting solution was centrifuged
Filter, obtains clear wax oil extracting solution；Repetitive operation 4 times, 5 batches of extracting solutions, total 9700L are collected altogether；
(2) it crosses chromatographic column: wax oil extracting solution obtained by step (1) is crossed into 500kgDX-7 resin column (production of Xi'an Lan Xiao resin processing plant),
Efflux after collecting upper prop, obtains chromatographic column collection liquid 10100L；
(3) concentrate abstraction impurity removal: being concentrated into 1500L for chromatographic column collection liquid obtained by step (2), be added 3000L petroleum ether or
Industrial hexane extracts 60 minutes, removes fat-soluble impurity, and petroleum ether or industrial hexane are recycled, degreasing concentrate is obtained
1500L；
(4) acid is adjusted in concentration: by chromatographic column collection liquid extracted obtained by step (3), it is molten that 33% food grade hydrochloric acid of mass concentration is added
Liquid adjusts pH value to 7, must neutralize solution 1550L；
(5) concentration is extracted: will be step (4) gained neutralization solution extraction 60 minutes using 3000L industrial hexane, coextraction 2 times, then
(thickening temperature is controlled at 70 DEG C or less) is concentrated under reduced pressure in extract liquor and is concentrated into 67L volume to get extraction concentrated liquor；
(5) crystallization filters: extraction concentrated liquor obtained by step (5) being stored at room temperature 12h crystallization, obtains dihydroartemisinic acid after suction filtration
Crude product 29.2kg；
(6) crude product refining: the pure methanol of 87L of dihydroartemisinic acid crude product 29.2kg obtained by step (6) is dissolved completely, crosses and filters out
Miscellaneous, concentration, crystallization filters, and washes crystalline substance, dry, obtain dihydroartemisinic acid finished product 26.8kg.
The present embodiment conversion ratio is 5.25%, obtained sampled detection (analysis means) its purity of dihydroartemisinic acid finished product
It is 99.4%.
Embodiment 4
The present embodiment the following steps are included:
(1) it extracts filtering: 100kg sweet wormwood wax oil, the methanol-water of 2000L70% and 12kg piece alkali being added in agitator tank and is stirred
It mixes, room temperature is extracted 4 hours, is stood to solution and is layered, takes supernatant to be filtered, obtain wax oil extracting solution, extracting solution was centrifuged
Filter, obtains clear wax oil extracting solution；Repetitive operation 4 times, 5 crowdes of extracting solution 9600L are collected altogether；
(2) it crosses chromatographic column: wax oil extracting solution obtained by step (1) is crossed into 500kgDX-7 resin column (production of Xi'an Lan Xiao resin processing plant),
Efflux after collecting upper prop, obtains chromatographic column collection liquid 10000L；
(3) concentrate abstraction impurity removal: being concentrated into 1500L for chromatographic column collection liquid obtained by step (2), be added 3000L petroleum ether or
Industrial hexane extracts 60 minutes, removes fat-soluble impurity, and petroleum ether or industrial hexane are recycled, degreasing concentrate is obtained
1500L；
(4) acid is adjusted in concentration: by degreasing concentrate obtained by step (3), 33% food grade salts acid solution of mass concentration is added, adjusts pH
Value must neutralize solution 1550L to 7；
(5) concentration is extracted: will be step (4) gained neutralization solution extraction 60 minutes using 3000L petroleum ether, coextraction 2 times, then will
Extract liquor is concentrated under reduced pressure (thickening temperature is controlled at 70 DEG C or less) and is concentrated into 60L volume to get extraction concentrated liquor；
(5) crystallization filters: extraction concentrated liquor obtained by step (5) being stored at room temperature 12h crystallization, obtains dihydroartemisinic acid after suction filtration
Crude product 27.9kg；
(6) crude product refining: the pure methanol of 86L of dihydroartemisinic acid crude product 27.9kg obtained by step (6) is dissolved completely, crosses and filters out
Miscellaneous, concentration, crystallization filters, and washes crystalline substance, dry, obtain 24.9 kg of dihydroartemisinic acid finished product.
The present embodiment conversion ratio is 4.98%, and obtained sampled detection ((HPLC)) its purity of dihydroartemisinic acid finished product is
99.3%。
Comparative example
This comparative example the following steps are included:
(1) dihydroartemisinic acid salt-forming reaction: 500 kilograms of wax oil in qinghaosu production process are taken, the 2%(M/ of 2500L is added
V) sodium bicarbonate aqueous solution is heated to 75 DEG C, after wax oil is in all molten condition, adjusts pH with saturated sodium bicarbonate aqueous solution
Value is 9, is stirred 30 minutes.It lets cool to room temperature, centrifugation, centrifugate 2350L；
(2) 600L petroleum ether and stirring extraction degreasing degreasing: will be added in centrifugate twice；
(3) hydrochloric acid is added after the aqueous alkali heating after degreasing being removed remaining petroleum ether, adjusts pH value to 5~6, puts
It is cooled to room temperature crystallization 12 hours, filters to obtain 31 kilograms of coarse-grain；
(4) recrystallize: recrystallization can obtain 23 kilograms of dihydroartemisinic acid product after crystal is dissolved with ethyl acetate.
The conversion ratio of the comparative example is that 4.6%, HPLC detection level is 98.6%.
In conclusion the method for extracting dihydroartemisinic acid from sweet wormwood wax oil of the present invention, advantage are that methanol energy is added
Enough preferably dissolution wax oils, wax oil is scatter, in favor of piece alkali by sweet wormwood wax oil dihydroartemisinic acid and piece alkali it is abundant
Haptoreaction generates more water-soluble double hydrogen Arteannuic acids and receives salt；It is more importantly chromatographed and (crosses resin column), resin column
There is no suction-operated to double hydrogen Arteannuic acids, but it is similar but be not saponified the terpene substances of removing to adsorb dihydroartemisinic acid structure, it is false
If do not removed these impurity, double hydrogen Arteannuic acids are when crystallization, due to making it difficult to by a large amount of other wax oil impurity package
Crystallization (crystallization needs to stand 24~48 hours), and crystallization not exclusively (is detected using HPLC, brilliant product proportion is precipitated and only has
More than 60%)；It improves water-soluble double hydrogen Arteannuic acids and receives the concentration of salt；Next after the methanol in recycling extracting solution, extractant is used
Extracting solution (alkalinity) after concentration is extracted oil-soluble impurity (such as pigment), gained concentrate by (petroleum ether or industrial hexane)
Acid adding tune pH to 5~7 makes its reaction regenerate dihydroartemisinic acid (oil-soluble), adds petroleum ether or industrial hexane to extract double
Hydrogen Arteannuic acid (oil-soluble) obtains extract liquor concentration, lets cool crystallization, and crystallization filters, and obtains the dihydroartemisinic acid crude product of high-content；
Then dihydroartemisinic acid crude product is only needed to refine once by recrystallizing methanol method, the dihydro sweet wormwood of high-purity can be obtained
Acid.
Claims (10)
1. a kind of method for extracting dihydroartemisinic acid from qinghaosu wax oil, which comprises the following steps:
(1) it extracts filtering: sweet wormwood wax oil, methanol, water and piece alkali being added in agitator tank and is stirred, stands to solution and is layered,
It takes supernatant to be filtered, obtains wax oil extracting solution；
(2) it crosses chromatographic column: wax oil extracting solution obtained by step (1) is crossed into resin column, the efflux after collecting upper prop obtains chromatographic column receipts
Liquid collecting；
(3) concentrate abstraction impurity removal: chromatographic column collection liquid obtained by step (2) is concentrated, concentrate is obtained；Be added extractant into
Row extraction, obtains degreasing concentrate；
(4) concentrate tune acid: by the resulting degreasing concentrate of step (3), acid solution is added and adjusts pH value, obtains neutralization solution；
(5) extraction concentration: extractant is added, is extracted, obtains extract liquor, then extract liquor is concentrated under reduced pressure, must extract
Take concentrated liquor；
(6) crystallization filters: extraction concentrate obtained by step (5) being stored at room temperature crystallization, dihydroartemisinic acid crude product is obtained after suction filtration；
(7) crude product refining: the methanol of dihydroartemisinic acid crude product obtained by step (6) is dissolved completely, filtering and impurity removing is concentrated, crystallization
It filters, washes crystalline substance, it is dry,.
2. the method for extracting dihydroartemisinic acid from qinghaosu wax oil according to claim 1, which is characterized in that step
(1) volumetric concentration for the methanol being added in is 50~80%, and dosage is 18~25 times of sweet wormwood wax oil.
3. the method for dihydroartemisinic acid is extracted from qinghaosu wax oil according to claim 2, which is characterized in that step
(1) volumetric concentration for the methanol being added in is 70%, and dosage is 20 times of sweet wormwood wax oil.
4. the method for dihydroartemisinic acid is extracted described according to claim 1~one of 3 from qinghaosu wax oil, which is characterized in that
In step (1), the dosage of the piece alkali of addition is 1/10~1/9 times of sweet wormwood wax oil.
5. the method for dihydroartemisinic acid is extracted described according to claim 1~one of 4 from qinghaosu wax oil, which is characterized in that
Agitator tank described in step (1) opens stirring before feeding intake, and starts timing after the completion of feeding intake, persistently stirs 4~12 hours.
6. the method for dihydroartemisinic acid is extracted described according to claim 1~one of 5 from qinghaosu wax oil, which is characterized in that
Chromatographic column collection liquid obtained by step (2) is concentrated into the 1/10~1/9 of original volume, obtains concentrate by step (3)；It is added opposite
It is extracted, is extracted 50~60 minutes in the extractant of 2~3 times of volumes of concentrate.
7. the method for dihydroartemisinic acid is extracted described according to claim 1~one of 6 from qinghaosu wax oil, which is characterized in that
In step (4), the acid solution is the hydrochloric acid solution of mass concentration 33%；PH value is adjusted to 5~7.
8. the method for dihydroartemisinic acid is extracted described according to claim 1~one of 7 from qinghaosu wax oil, which is characterized in that
Extractant described in step (3) and step (5) is the petroleum ether or industrial hexane that boiling range is 60~90 DEG C.
9. the method for dihydroartemisinic acid is extracted described according to claim 1~one of 8 from qinghaosu wax oil, which is characterized in that
In step (5), it is added and is equivalent to the extractant that step (4) gained neutralizes 2~4 times of volumes of solution, continuous extraction 2~3 times；Extraction
Liquid is taken to be concentrated under reduced pressure into the 1/4~1/3 of original volume；Thickening temperature is controlled at 70 DEG C of <.
10. the method for dihydroartemisinic acid is extracted described according to claim 1~one of 9 from qinghaosu wax oil, which is characterized in that
In step (7), the volume for dissolving methanol used in dihydroartemisinic acid crude product is 2~4 times of dihydroartemisinic acid crude product volume.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110623002A (en) * | 2019-09-18 | 2019-12-31 | 禹州市天源生物科技有限公司 | Preparation method of sweet wormwood wax oil insect repellent |
| CN111533653A (en) * | 2020-06-02 | 2020-08-14 | 禹州市天源生物科技有限公司 | Method for separating and purifying dihydroartemisinic acid from artemisinin waste wax oil |
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