CN104788532A - Extraction preparation method of triptolide - Google Patents
Extraction preparation method of triptolide Download PDFInfo
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- CN104788532A CN104788532A CN201510213692.2A CN201510213692A CN104788532A CN 104788532 A CN104788532 A CN 104788532A CN 201510213692 A CN201510213692 A CN 201510213692A CN 104788532 A CN104788532 A CN 104788532A
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- triptolide
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- C07J—STEROIDS
- C07J73/00—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms
- C07J73/001—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms by one hetero atom
- C07J73/003—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms by one hetero atom by oxygen as hetero atom
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Abstract
The invention provides an extraction preparation method of triptolide. The method comprises the steps of extracting thunder god vine herbs by utilizing ethyl acetate, dissolving extract by utilizing dichloromethane, then carrying out the alkali wash, carrying out the secondary positive silica-gel column chromatography, carrying out the elution sequentially by utilizing dichloromethane, dichloromethane/methanol mixed solvent and methanol for the primary column chromatography, carrying out the gradient elution by utilizing petroleum ether/ethyl acetate mixed solvent for the secondary column chromatography, and finally preparing a triptolide pure product in a crystallizing manner. The preparation method is fewer in steps and simple to operate, the triptolide product with high purity can be effectively obtained, and the production cost of the triptolide can be greatly reduced.
Description
Technical field
The present invention relates to a kind of extraction preparation method of triptolide, belong to medical art.
Background technology
Trypterygine (Tripterygium wilfordii Hook f.) is Celastraceae tripterygium plant, Chinese medicine voluminous dictionary is recorded, have dispel rheumatism, remove obstruction in channels to relieve pain, effect of swelling and pain relieving, removing toxic substances desinsection, clinically be used for the treatment of the autoimmune disorders such as rheumatoid arthritis, chronic nephritis and lupus erythematosus, in recent years for the antirejection therapy of organ transplantation, all achieve good therapeutic effect.Modern study finds that trypterygine has the effects such as anti-inflammatory, anti-immunity, antifertility, antitumor, anti-microbial activity in succession.So far from trypterygine, isolated 200 number of chemical monomers, wherein diterpenes, sesquiterpene alkaloids class, triterpenes are main active ingredient.
Triptolide (triptolide) is the epoxidation diterpenic lactone that isolated activity is the highest from trypterygine, is one of principle active component of trypterygine, and its relevant potency ratio tripterygium preparation height 100-200 doubly.Show through pharmacology and clinical trial, it has definite immunosuppression, anti-inflammatory, antifertility and the biological activity such as antitumor.
But the content of triptolide in trypterygine is very low, the yield of its extraction and isolation is also very low, and according to the literature, plant is separated yield and is only 0.001% (w/w).
The preparation technology of triptolide crude extract mainly contains alcohol reflux-neutral alumina absorption-chloroform extraction, alcohol reflux-chloroform extraction, alcohol reflux-extraction into ethyl acetate and water boiling and precipitation with ethanol-acetic acid ethyl ester or chloroform extraction etc., and in the trichloromethane medicinal extract of gained, the content of triptolide is about 0.23%.CN101434638A provides a kind of method extracting triptolide crude product from trypterygine, adopts chloride alkane to carry out pressurised extraction, obtains triptolide crude product, purity about 1% after extracting solution concentrating under reduced pressure.
CN101367862 discloses a kind of method of separating high-purity triptolide from trypterygine, carry out heat with alcohol to medicinal material to carry, gained alcohol extract first uses petroleum ether extraction, then with chloroform or dichloromethane extraction, on chloroform or dichloromethane extract, aluminum oxide or silicagel column carry out column chromatography, with chloroform/methanol or methylene chloride/methanol mixed solvent wash-out, the cut of Fractional Collections is gone up high performance preparative liquid chromatography again and obtains triptolide work in-process, finally crystallization obtains triptolide sterling in organic solvent.
CN103524591A discloses a kind of method taking tripterygium root as raw material and extract triptolide: the ethanol-extracted medicinal extract of tripterygium root is distributed in the double-aqueous phase system formed by polymerinorganic salt brine solution and ethanol, then extracting being distributed in trypterygine medicinal extract in double-aqueous phase system by water-insoluble organic solvents, obtaining efficient part.The efficient part alcohol obtained is dissolved, adds the efficient part that the most of non-effective material of water crystallization removing obtains enrichment.The efficient part of this enrichment is separated through silica gel column chromatography, obtains triptolide after recrystallization.
Current triptolide extracting and purifying method ubiquity crude extract triptolide accumulation rate is low, purifying process is complicated, length consuming time, efficiency are low, yield is low, high in cost of production defect.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides the novel method that a kind of triptolide extracts preparation, greatly can simplify production technique and enhance productivity, improve triptolide recovery rate.
The technical solution used in the present invention is:
There is provided a kind of extraction preparation method of triptolide, it comprises the steps:
(1) extract: tripterygium wilfordii is crushed to 20 ~ 30 orders, extract 2 ~ 3 times, each 4 ~ 8 hours by 5 ~ 15 times amount (weight) ethyl acetate backflow, after filtering, concentrated extracting solution obtains the medicinal extract that weight is tripterygium wilfordii weight 2 ~ 3%;
(2) alkali cleaning: with 0.2 ~ 0.8moL/L NaOH solution washing 2 ~ 3 times after medicinal extract is dissolved with methylene dichloride, concentrated methylene dichloride mutually must medicinal extract after alkali cleaning;
(3) first time column chromatography: by normal phase silicagel column on medicinal extract after alkali cleaning, first use dichloromethane eluent, the thin out rear methylene chloride/methanol mixed solvent wash-out of wash water color 1 ~ 2 column volume, then use methanol-eluted fractions, concentrated meoh eluate obtains methanol-eluted fractions thing;
(4) second time column chromatography: methanol-eluted fractions thing is gone up normal phase silicagel column again, gradient elution is carried out with petrol ether/ethyl acetate mixed solvent, collect the elutriant containing triptolide, leave standstill crystallization after being concentrated into 1/4 ~ 1/10 times of volume, obtain triptolide crude product;
(5) sterling preparation: leave standstill crystallization by after triptolide crude product organic solvent dissolution, filter out crystal and obtain triptolide sterling.
Optionally, the xitix of medicinal material weight 0.05 ~ 0.15% can be added during step (1) refluxing extraction.
In one embodiment, the consumption of step (2) described methylene dichloride is per kilogram medicinal material methylene dichloride 0.5 ~ 1.5 liter, and each alkali cleaning NaOH solution consumption is 0.5 ~ 1.6 times (volume) of methylene dichloride.
In one embodiment, step (3) column chromatography adopts 200 ~ 300 order purification on normal-phase silica gel, consumption is 2 ~ 10 times of medicinal extract weight, and adopt the mode of Shi Fa Installed post, described mixed solvent is methylene dichloride: the mixed solvent of methyl alcohol=80 ~ 10:1 (volume ratio).
In one embodiment, step (4) column chromatography adopts 200 ~ 300 order purification on normal-phase silica gel, consumption is 20 ~ 60 times of medicinal extract weight, the Cai mode of Gan Fa Installed post or Shi Fa Installed post, described mixed solvent is sherwood oil: the mixed solvent of ethyl acetate=10 ~ 1:1 (volume ratio).
In one embodiment, the described gradient elution mode of step (4) is for use sherwood oil successively: the mixed solvent wash-out of ethyl acetate=10:1,6:1,4:1,2:1,1:1 (volume ratio), each ratio wash-out 3 ~ 10 column volumes.
In one embodiment, step (5) described organic solvent is selected from following solvent system: sherwood oil/methylene dichloride, petrol ether/ethyl acetate, sherwood oil/acetone, isopropyl ether.
In one embodiment, the temperature of step (4), (5) described standing crystallization is 4 DEG C or room temperature.
The preparation method of column chromatography of the present invention sample to be separated: q. s. methylene chloride dissolves medicinal extract, adds whip attachment in appropriate 80 order purification on normal-phase silica gel, grinds loose uniformly grains of sand shape and get final product after about 50 DEG C of reduction vaporizations fall organic solvent.
The preferred triptolide content of tripterygium wilfordii of the present invention is greater than the medicinal material of 30ppm (namely 0.003%), compared with low levels medicinal material, identical cost consumption can obtain the triptolide product of more, contribute to the production cost reducing unit product better, increase economic efficiency.
The content assaying method of triptolide in medicinal material: get 50g pulverizing medicinal materials to 20 ~ 30 order, extracts 2 times with 20 times of methanol eddies, each 4 hours, concentrated after extracting liquid filtering, is settled to 50mL as need testing solution with dissolve with methanol; Get triptolide reference substance appropriate, accurately weighed, add dissolve with methanol and make the solution in contrast product solution of every 1mL containing 50 μ g; HPLC chromatographic condition: chromatographic column: phenomenex C
18(4.6mm × 250mm, 5 μm); Moving phase: A: methyl alcohol, B: methanol-water (40:60); Flow velocity: 0.9mL/min, according to the form below carries out gradient elution:
Triptolide condition of gradient elution
Determined wavelength 218nm, column temperature 25 DEG C, sample size 10 μ L.
Triptolide provided by the invention extracts preparation method and has the following advantages:
(1) step is few, easy and simple to handle.
(2) medicinal material directly avoids other large polar component with ethyl acetate extraction and is extracted generation interference, decreases medicinal extract treatment capacity, simplifies follow-up work amount, improve extraction and isolation efficiency.
(3) caustic scrubbing step eliminates most of impurity rapidly, triptolide is enriched in after alkaline purification in medicinal extract effectively, thus ensure that subsequent columns chromatographic step can obtain highly purified triptolide product with high yield.
(4) simplify operation steps, greatly reduce triptolide production cost.
Embodiment
Below will the invention will be further described by embodiment, these descriptions are not be further limited content of the present invention.One skilled in the art will understand that the equivalent replacement that content of the present invention is done, or improve accordingly, still belong within protection scope of the present invention.
Embodiment 1
Tripterygium wilfordii 300 kilograms (after testing, its triptolide content is 0.0043%), be crushed to 20 ~ 30 orders, load extractor, add 3 tons of ethyl acetate, then add 360g xitix, heating and refluxing extraction 3 times, each 5 hours, extracting solution after filtration, concentrating under reduced pressure obtains medicinal extract 8.3 kilograms; Dissolve medicinal extract with 360 liters of methylene dichloride, squeeze into extractor, separately take 17.28 kilograms of NaOH, prepare 720 liters of 0.6moL/L NaOH solution, point squeeze into extractor 2 times, carry out alkali cleaning 2 times to methylene dichloride lysate, concentrated methylene dichloride mutually must medicinal extract 2 kilograms after alkali cleaning; Get 10 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Shi Fa Installed diameter 35cm post, first dichloromethane eluent is used after medicinal extract loading after alkali cleaning, with methylene dichloride after wash water color is thin out: methyl alcohol=50:1 mixed solvent wash-out 2 column volumes, then use methanol-eluted fractions, concentrated meoh eluate obtains methanol-eluted fractions thing 427g; Get 20 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Shi Fa Installed diameter 50cm post, sherwood oil is used successively: the mixed solvent of ethyl acetate=10:1,6:1,4:1,2:1,1:1 (volume ratio) carries out gradient elution after methanol-eluted fractions thing loading, each ratio wash-out about 8 column volumes, collect the elutriant containing triptolide, leave standstill crystallization at 4 DEG C after being concentrated into about 1/8 volume, obtain triptolide crude product 13.8g; Crude product isopropyl ether is made recrystallisation solvent and at room temperature carries out recrystallization, filter after crystallization triptolide sterling 12.3g, HPLC to detect its purity be 99.4%.
Embodiment 2
Tripterygium wilfordii 200 kilograms, is crushed to 20 ~ 30 orders, loads extractor, adds 3 tons of ethyl acetate, heating and refluxing extraction 2 times, each 4 hours, and extracting solution after filtration, concentrating under reduced pressure obtains medicinal extract 6.0 kilograms; Dissolve medicinal extract with 300 liters of methylene dichloride, squeeze into extractor, separately take 14.4 kilograms of NaOH, prepare 450 liters of 0.8moL/L NaOH solution, point squeeze into extractor 3 times, alkali cleaning carried out 3 times to methylene dichloride lysate, concentrated methylene dichloride mutually medicinal extract 1.2 kilograms after alkali cleaning; Get 12 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Shi Fa Installed diameter 35cm post, first dichloromethane eluent is used after medicinal extract loading after alkali cleaning, with methylene dichloride after wash water color is thin out: methyl alcohol=10:1 mixed solvent wash-out 2 column volumes, then use methanol-eluted fractions, concentrated meoh eluate obtains methanol-eluted fractions thing 304g; Get 18 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Gan Fa Installed diameter 50cm post, sherwood oil is used successively: the mixed solvent of ethyl acetate=6:1,4:1,2:1,1:1 (volume ratio) carries out gradient elution after methanol-eluted fractions thing loading, each ratio wash-out about 10 column volumes, collect the elutriant containing triptolide, leave standstill crystallization at 4 DEG C after being concentrated into about 1/10 volume, obtain triptolide crude product 8.7g; Crude product petrol ether/ethyl acetate mixed solvent is made recrystallisation solvent and at room temperature carries out recrystallization, filter after crystallization triptolide sterling 7.5g, HPLC to detect its purity be 99.8%.
Embodiment 3
Tripterygium wilfordii 250 kilograms (after testing, its triptolide content is 0.0039%), be crushed to 20 ~ 30 orders, load extractor, add 2.5 tons of ethyl acetate, then add 375g xitix, heating and refluxing extraction 2 times, each 4 hours, extracting solution after filtration, concentrating under reduced pressure obtains medicinal extract 6.3 kilograms; Medicinal extract is dissolved with 220 liters of methylene dichloride, squeeze into extractor, separately take 4.8 kilograms of NaOH, prepare 240 liters of 0.5moL/L NaOH solution, divide and squeeze into extractor 2 times, first time 130 liters, second time 110 liters, alkali cleaning is carried out 2 times to methylene dichloride lysate, concentrated methylene dichloride mutually medicinal extract 1.6 kilograms after alkali cleaning; Get 6 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Shi Fa Installed diameter 20cm post, first dichloromethane eluent is used after medicinal extract loading after alkali cleaning, with methylene dichloride after wash water color is thin out: methyl alcohol=80:1 mixed solvent wash-out 1 column volume, then use methanol-eluted fractions, concentrated meoh eluate obtains methanol-eluted fractions thing 349g; Get 11 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Gan Fa Installed diameter 40cm post, sherwood oil is used successively: the mixed solvent of ethyl acetate=6:1,4:1,2:1,1:1 (volume ratio) carries out gradient elution after methanol-eluted fractions thing loading, each ratio wash-out about 5 column volumes, collect the elutriant containing triptolide, be concentrated into left at room temperature crystallization after about 1/6 volume, obtain triptolide crude product 10.2g; Crude product sherwood oil/acetone mixed solvent is made recrystallisation solvent and at room temperature carries out recrystallization, filter after crystallization triptolide sterling 9.1g, HPLC to detect its purity be 99.6%.
Embodiment 4
Tripterygium wilfordii 350 kilograms (after testing, its triptolide content is 0.003%), is crushed to 20 ~ 30 orders, load extractor, add 1.8 tons of ethyl acetate, heating and refluxing extraction 3 times, each 8 hours, extracting solution after filtration, concentrating under reduced pressure obtains medicinal extract 9.2 kilograms; Dissolve medicinal extract with 175 liters of methylene dichloride, squeeze into extractor, separately take 2.16 kilograms of NaOH, prepare 270 liters of 0.2moL/LNaOH solution, divide equally 3 times and squeeze into extractor, alkali cleaning is carried out 3 times to methylene dichloride lysate, concentrated methylene dichloride mutually medicinal extract 2.1 kilograms after alkali cleaning; Get 4.2 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Shi Fa Installed diameter 20cm post, first dichloromethane eluent is used after medicinal extract loading after alkali cleaning, with methylene dichloride after wash water color is thin out: methyl alcohol=10:1 mixed solvent wash-out 1 column volume, then use methanol-eluted fractions, concentrated meoh eluate obtains methanol-eluted fractions thing 458g; Get 9.2 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Shi Fa Installed diameter 40cm post, sherwood oil is used successively: the mixed solvent of ethyl acetate=10:1,6:1,4:1,2:1,1:1 (volume ratio) carries out gradient elution after methanol-eluted fractions thing loading, each ratio wash-out about 3 column volumes, collect the elutriant containing triptolide, be concentrated into left at room temperature crystallization after about 1/4 volume, obtain triptolide crude product 11.4g; Crude product sherwood oil/methylene dichloride mixed solvent is made recrystallisation solvent and at room temperature carries out recrystallization, filter after crystallization triptolide sterling 9.5g, HPLC to detect its purity be 99.3%.
Embodiment 5
Tripterygium wilfordii 250 kilograms (after testing, its triptolide content is 0.0022%), be crushed to 20 ~ 30 orders, load extractor, add 3 tons of ethyl acetate, then add 250g xitix, heating and refluxing extraction 2 times, each 6 hours, extracting solution after filtration, concentrating under reduced pressure obtains medicinal extract 6.7 kilograms; Dissolve medicinal extract with 200 liters of methylene dichloride, squeeze into extractor, separately take 9 kilograms of NaOH, prepare 450 liters of 0.5moL/L NaOH solution, divide and squeeze into extractor 3 times, each 150 liters, alkali cleaning is carried out 3 times to methylene dichloride lysate, concentrated methylene dichloride mutually medicinal extract 1.4 kilograms after alkali cleaning; Get 8 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Shi Fa Installed diameter 30cm post, first dichloromethane eluent is used after medicinal extract loading after alkali cleaning, with methylene dichloride after wash water color is thin out: methyl alcohol=30:1 mixed solvent wash-out 1 column volume, then use methanol-eluted fractions, concentrated meoh eluate obtains methanol-eluted fractions thing 318g; Get 12 kilogram of 200 ~ 300 order Qingdao Haiyang column chromatography purification on normal-phase silica gel Gan Fa Installed diameter 40cm post, sherwood oil is used successively: the mixed solvent of ethyl acetate=6:1,4:1,2:1,1:1 (volume ratio) carries out gradient elution after methanol-eluted fractions thing loading, each ratio wash-out about 6 column volumes, collect the elutriant containing triptolide, leave standstill crystallization at 4 DEG C after being concentrated into about 1/4 volume, obtain triptolide crude product 6.4g; Crude product isopropyl ether is made recrystallisation solvent and at room temperature carries out recrystallization, filter after crystallization triptolide sterling 5.0g, HPLC to detect its purity be 99.7%.
Claims (9)
1. an extraction preparation method for triptolide, is characterized in that comprising the steps:
(1) extract: tripterygium wilfordii is crushed to 20 ~ 30 orders, extract 2 ~ 3 times, each 4 ~ 8 hours by 5 ~ 15 times amount (weight) ethyl acetate backflow, after filtering, concentrated extracting solution obtains the medicinal extract that weight is tripterygium wilfordii weight 2 ~ 3%;
(2) alkali cleaning: with 0.2 ~ 0.8moL/L NaOH solution washing 2 ~ 3 times after medicinal extract is dissolved with methylene dichloride, concentrated methylene dichloride mutually must medicinal extract after alkali cleaning;
(3) first time column chromatography: by normal phase silicagel column on medicinal extract after alkali cleaning, first use dichloromethane eluent, the thin out rear methylene chloride/methanol mixed solvent wash-out of wash water color 1 ~ 2 column volume, then use methanol-eluted fractions, concentrated meoh eluate obtains methanol-eluted fractions thing;
(4) second time column chromatography: methanol-eluted fractions thing is gone up normal phase silicagel column again, gradient elution is carried out with petrol ether/ethyl acetate mixed solvent, collect the elutriant containing triptolide, leave standstill crystallization after being concentrated into 1/4 ~ 1/10 times of volume, obtain triptolide crude product;
(5) sterling preparation: leave standstill crystallization by after triptolide crude product organic solvent dissolution, filter out crystal and obtain triptolide sterling.
2. the extraction preparation method of triptolide as claimed in claim 1, adds the xitix of medicinal material weight 0.05 ~ 0.15% when it is characterized in that step (1) refluxing extraction.
3. the extraction preparation method of triptolide as claimed in claim 1 or 2, it is characterized in that the consumption of step (2) described methylene dichloride is per kilogram medicinal material methylene dichloride 0.5 ~ 1.5 liter, each alkali cleaning NaOH solution consumption is 0.5 ~ 1.6 times (volume) of methylene dichloride.
4. the extraction preparation method of triptolide as claimed in claim 1 or 2, it is characterized in that step (3) column chromatography adopts 200 ~ 300 order purification on normal-phase silica gel, consumption is 2 ~ 10 times of medicinal extract weight, adopt the mode of Shi Fa Installed post, described mixed solvent is methylene dichloride: the mixed solvent of methyl alcohol=80 ~ 10:1 (volume ratio).
5. the extraction preparation method of triptolide as claimed in claim 1 or 2, it is characterized in that step (4) column chromatography adopts 200 ~ 300 order purification on normal-phase silica gel, consumption is 20 ~ 60 times of medicinal extract weight, the Cai mode of Gan Fa Installed post or Shi Fa Installed post, described mixed solvent is sherwood oil: the mixed solvent of ethyl acetate=10 ~ 1:1 (volume ratio).
6. the extraction preparation method of triptolide as claimed in claim 5, it is characterized in that the described gradient elution mode of step (4) is for use sherwood oil successively: the mixed solvent wash-out of ethyl acetate=10:1,6:1,4:1,2:1,1:1 (volume ratio), each ratio wash-out 3 ~ 10 column volumes.
7. the extraction preparation method of triptolide as claimed in claim 1 or 2, is characterized in that step (5) described organic solvent is selected from following solvent system: sherwood oil/methylene dichloride, petrol ether/ethyl acetate, sherwood oil/acetone, isopropyl ether.
8. the extraction preparation method of triptolide as claimed in claim 1 or 2, is characterized in that step (4), the temperature of (5) described standing crystallization is 4 DEG C or room temperature.
9. the extraction preparation method of the triptolide as described in any one of claim 1 ~ 8, is characterized in that, described tripterygium wilfordii is the medicinal material that triptolide content is greater than 30ppm.
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| CN105348366A (en) * | 2015-12-11 | 2016-02-24 | 许志强 | Extracting method for triptolide |
| CN109021061A (en) * | 2018-09-29 | 2018-12-18 | 郭可点 | Triptolide targeted prodrug and its preparation method and application |
| CN112574182A (en) * | 2020-10-12 | 2021-03-30 | 江西中医药大学 | Effective part of tripterygium wilfordii macrocyclic polyamine alkaloid and preparation method thereof |
| CN115073278A (en) * | 2022-07-20 | 2022-09-20 | 江苏知原药业股份有限公司 | Method for extracting tripterygium wilfordii paraquinone B from tripterygium wilfordii |
| CN115894602A (en) * | 2022-12-24 | 2023-04-04 | 浙江得恩德制药股份有限公司 | Extraction of triptolide from tripterygium wilfordii |
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| CN109021061A (en) * | 2018-09-29 | 2018-12-18 | 郭可点 | Triptolide targeted prodrug and its preparation method and application |
| CN109021061B (en) * | 2018-09-29 | 2019-07-12 | 郭可点 | Triptolide targeted prodrug and its preparation method and application |
| CN112574182A (en) * | 2020-10-12 | 2021-03-30 | 江西中医药大学 | Effective part of tripterygium wilfordii macrocyclic polyamine alkaloid and preparation method thereof |
| CN112574182B (en) * | 2020-10-12 | 2023-08-04 | 江西中医药大学 | Tripterygium wilfordii macrocyclic polyamine alkaloid effective part and preparation method thereof |
| CN115073278A (en) * | 2022-07-20 | 2022-09-20 | 江苏知原药业股份有限公司 | Method for extracting tripterygium wilfordii paraquinone B from tripterygium wilfordii |
| CN115894602A (en) * | 2022-12-24 | 2023-04-04 | 浙江得恩德制药股份有限公司 | Extraction of triptolide from tripterygium wilfordii |
| CN115894602B (en) * | 2022-12-24 | 2024-05-14 | 浙江得恩德制药股份有限公司 | Extraction of triptolide from Tripterygium wilfordii |
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Denomination of invention: A Method for Extracting and Preparing Triptolide A Effective date of registration: 20230328 Granted publication date: 20160622 Pledgee: Bank of China Limited Chengdu Wuhou sub branch Pledgor: AKTIN CHEMICALS Inc. Registration number: Y2023510000084 |