CN1911932A - Method for separating preparing tripterygium wilfordii monomer from tripterygium wilfordii by countercurrent flow chromatography - Google Patents
Method for separating preparing tripterygium wilfordii monomer from tripterygium wilfordii by countercurrent flow chromatography Download PDFInfo
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Abstract
The countercurrent chromatographic process for separating and preparing tripterygium alkaloid monomer from tripterygium material includes the following steps: 1. extracting crude total tripterygium alkaloid, mixing crude total tripterygium alkaloid with methanol, filtering to obtain filter residue and drying, and re-crystallizing in methanol to obtain total tripterygium alkaloid; 2. compounding the fixed phase and the flowing phase of two-phase solvent system; 3. filling the column of countercurrent chromatograph with the fixed phase; 4.pumping the flowing phase into the column of the high speed countercurrent chromatograph; and 5. feeding the total tripterygium alkaloid and collecting different tripterygium alkaloid monomers based on the detector spectral graph. The present invention can obtain different tripterygium alkaloid monomers in purity over 95 %.
Description
Technical field
The present invention relates to a kind of counter current chromatography and from trypterygine, separate the method for preparing the trypterygine alkaloid monomer.
Background technology
Trypterygine (Tripterygium wilfordii Hook.f. (Celastraceae, TWHF)) be Chinese a kind of traditional Chinese medicine, mainly be distributed in south China one band, have effect (C.N.Liu, M.Peng, Anticancer Chinese Herb Dictionary such as treatment Immunological diseases, anti-inflammatory, antifertility, Science andTechnology Publishing Co., Hubei, 1994, p.1072).Main effectively activeconstituents is trypterygine alkaloid, diterpene and triterpene compound (Qian Shao Zhen in the trypterygine, Xu Ye, Zhangjian Wei.Recent progress in research Tripterygium:A male antiferilityplant, Contraception, 1995,51:121-129).Wilforgine 20 (wilforgine), Wilforine (wilforine), wilfordine (wilfordine), wilfortrine (wilfortrine) are to separate (Beroza M.Alkaloids from Tripterygiumwilfordii Hook.The structure of wilforine in tripterygium root the earliest, wilfordine, wilforgine, wilfortrine.J Amer.Chem.Soc., 1953,75:44-49.)。
The trypterygine alkaloid has purposes widely, can be used as sterilant (Luo Douqiang, Feng Juntao, Hu a ceremonial jade-ladle, used in libation, Zhu Mujin, Zhang Xing, the tripterygium total alkaloid separates and insecticidal activity research, Xibei Univ. of Agricultural ﹠ Forest Science ﹠ Technology's journal (natural science edition), 2001,29 (2) 61-64), also can be used as plant amedica and carry out screening active ingredients.All contain this several trypterygine alkaloids in every kind of trypterygine prepared slices of Chinese crude drugs, wilfortrine and Wilforine have humoral immunization suppress effect (Wang Cuidi, Guo Yupu, the effective constituent of trypterygine, pharmacological action and clinical effect. Chinese combination of Chinese tradiational and Western medicine magazine, 1993,13 (8): 507; Zheng Jiarun, the toxicity research of tripterygium total glycosides. Chinese Academy of Medical Sciences's journal, 1987,9 (5): 323).Wherein wilfortrine has anti HIV-1 virus effect (Hong quan Duan et al, J.Nat.Prod.2000,63,357-361) and immunosuppressive action (Zheng Youlan, Xu Ya, the immunosuppressive action of wilfortrine and Euonine, Acta Pharmaceutica Sinica, 1989,24 (8) 568-572) Wilforine has and suppresses leukemia and get effect (The structure oftriptodihydroxy acid methyl ester and wilfortrine.Deng, Fu xiao, Cao, Jian hong, Xia, Zhi lin, Lin, Sui, Wang, Xiao yi, Zhi wu xue bao (1987), 29 (1), 73-6.; Zheng Y.L., Xu Y., Lin J.F., Acta pharmaceutica Sinica (1989), 24 (8), 568-72).The quality monitoring of pharmacology, drug research and the trypterygine prepared slices of Chinese crude drugs all needs a large amount of alkaloid monomers, the trypterygine alkaloid is the object that people study always, a lot of documents has all been reported tripterygium total alkaloid extraction method (Chen Junyuan, Xia Zhilin, Deng Fuxiao. the improvement of trypterygine alkaloid extracting technique, Chinese Journal of Pharmaceuticals, 1989,20 (11) 484-485).Existing bibliographical information adopts the method for column chromatography to separate, but purity is not high, and the rate of recovery is very low.High speed adverse current chromatogram (High-speedcountercurrent chromatography, HSCCC) be that a kind of successive that grew up in recent years need not the efficient of any solid support, liquid liquid divides color matching to say isolation technique fast, it avoided variety of issue that solid state adhesion body or carrier bring as: sample easily is adsorbed, loss and sex change, when using other liquid phase chromatography amount of being prepared to separate, its allocative efficiency can obviously reduce, solvent-oil ratio is big, HSCCC guarantees higher peak shape resolution, fractional dose is bigger, sample loss is few, the yield height, isolating environment relaxes, and saves solvent.Counter current chromatograph can directly advance relatively large product or the synthetic mixture of slightly getting sample, and separating resulting can reach quite high purity, has been widely used in the preparation separation and the purifying of field chemical substances such as biology, medicine, environmental protection.
Summary of the invention
The present invention relates to a kind of counter current chromatography and from trypterygine, separate the method for preparing the trypterygine alkaloid monomer.
The step of method is as follows:
1) trypterygine radical center, the dry pulverizing of root skin or stem, use ethanol percolation, the ethanolic soln extracting solution that diafiltration obtains is evaporated to the dried ethanol extract that obtains, ethanol extract chloroform extraction 3～6 times, obtain chloroform medicinal extract, chloroform medicinal extract is 8-11 with 3～6 after-filtration of acid extraction of mass percent concentration 4-20%, filtrate with alkali adjusting pH value, separates out solid, filter back deionized water wash 3～6 times, oven dry obtains thick total alkaloids, and thick total alkaloids is added the methyl alcohol mixing, filter, collect filter residue, drying obtains pure total alkaloids with recrystallizing methanol, is used for high speed adverse current chromatogram separation raw material;
3) with volume ratio be the alkane of 1-6: 1-7: 1-5: 1-8: fatty ester: Fatty Alcohol(C12-C14 and C12-C18): water preparation high speed adverse current chromatogram two-phase solvent system, place separating funnel, shake up, standing demix, after the balance, separate mutually upper and lower;
4) use the phase that fixes mutually, make moving phase mutually down, use the chromatogram pillar that is full of mutually in the whole counter current chromatograph, adjusting the counter current chromatograph main frame just changes, following phase moving phase pumped into from the head end of pillar carries out wash-out in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction; Perhaps with down as stationary phase, on make moving phase mutually, be full of whole adverse current chromatogram pillar mutually with following, the adjustment main frame is just changeing, and last phase moving phase is pumped into from the tail end of pillar carry out wash-out in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction; Spectrogram according to detector is collected target compound step by step, and concentrating under reduced pressure obtains each alkaloid monomer crude product, obtains wilfortrine, wilfordine, Wilforgine 20, Wilforine respectively through recrystallizing methanol again.
Advantage of the present invention is: used trypterygine is widely distributed in China, so raw material of the present invention is easy to get; Used various chemical reagent is all very common, easily mass purchase; This separation process can be carried out continuously, and is easy and simple to handle, the efficient height, and wilfortrine, wilfordine, Wilforgine 20, Wilforine purity are greater than 95%; Compare with column chromatography isochromatic spectrum method, it need not any solid-state upholder or carrier, therefore the sample absorption loss that does not have solid-state carrier and caused, stain and problem such as sex change, be a kind of economy from the trypterygine crude extract, separate the method for preparing wilfortrine, wilfordine, Wilforgine 20, Wilforine; Can directly advance relatively large tripterygium total alkaloid; The counter current chromatograph that is suitable for various models separates preparation wilfortrine, wilfordine, Wilforgine 20, Wilforine.
The present invention is described further below in conjunction with embodiment and accompanying drawing
Description of drawings
Fig. 1 is the pure total alkaloids high speed adverse current chromatogram of the trypterygine of embodiment 1,3 (HSCCC) separate colors spectrogram;
Fig. 2 is the pure total alkaloids high speed adverse current chromatogram of the trypterygine of embodiment 2,4 (HSCCC) separate colors spectrogram;
Among the figure: a, b, c, d are respectively the adverse current chromatogram peak of wilfortrine, wilfordine, Wilforgine 20 and Wilforine;
Fig. 3 is the high performance liquid phase detection figure of wilfortrine of the present invention;
Fig. 4 is the high performance liquid phase detection figure of Wilforgine 20 of the present invention;
Fig. 5 is the high performance liquid phase detection figure of wilfordine of the present invention;
Fig. 6 is the high performance liquid phase detection figure of Wilforine of the present invention;
Fig. 7 is the high performance liquid phase detection figure of the pure total alkaloids of trypterygine of the present invention.
Embodiment
Embodiment 1:
1, the 10kg velamen of Tripterygium wilfordii is used 30L 60% ethanol percolation 10 hours, collect percolate, concentrating under reduced pressure obtains ethanol extract, ethanol extract is with chloroform extraction 3 times, and the chloroform medicinal extract that concentrating under reduced pressure obtains is with 4% hydrochloric acid extraction 6 times, filtering and collecting filter liquid, it is between the 8-11 that filtrate is regulated the pH value with sodium hydroxide, separate out solid, filter back solid deionized water wash 3 times, obtain thick total alkaloids 30g behind the solid drying.
2, thick total alkaloids fully dissolves with 200mL methyl alcohol, filters and collects filter residue, and filter residue obtains pure total alkaloids 10g with the crystallization of methyl alcohol thermosol.
3, separate pure total alkaloids with high-speed counter-current chromatograph (TBE-1000A is produced with the biochemical company limited in field in Shanghai), the high performance liquid phase of pure total alkaloids detects color atlas as shown in Figure 7.
1) applied sample amount 700mg adopts normal hexane: ethyl acetate: ethanol: water=6: 4: 5: the solvent systems of 8 (v/v/v/v); Column volume 1000mL, rotating speed are 500rpm, 25 ℃ of column temperatures, below be stationary phase mutually, be moving phase mutually down, flow velocity 5mL/min, the stationary phase retention value of system is 72%, ultraviolet detection wavelength 254nm, detected result is seen accompanying drawing 1, a, b, c, d are respectively the adverse current chromatogram peak of wilfortrine, wilfordine, Wilforgine 20 and Wilforine.
2) operation steps is: at first place separating funnel by above-mentioned volume ratio preparation solvent systems, after shaking up, standing demix, isoequilibrium separated mutually with upper and lower after for some time.Then, use earlier as stationary phase, be full of whole pillar, adjust main frame and just change, rotating speed is 500rmp, will descend phase moving phase to pump in the post from the head end of pillar with the flow velocity of 5.0mL/min; After treating that whole system is set up running balance, go up the pure total alkaloids raw material of phased soln 700mg with 40mL, by the sampling valve sample introduction; Collect target compound according to the detector spectrogram then, obtain wilfortrine 85mg, wilfordine 95mg, Wilforgine 20 215mg, Wilforine 200mg respectively through recrystallizing methanol.High performance liquid phase check and analysis condition: chromatographic column is Zorbax SB C-18HPLC post (250mm * 4.6mm i.d, 5 μ m, Agilent), 35 ℃ of column temperatures, moving phase is acetonitrile: water=55: 45 (v/v), flow velocity 0.8mL/min, ultraviolet detection wavelength 254nm detect gained alkaloid monomer purity, the results are shown in accompanying drawing 3-6.
Embodiment 2:
1, the 10kg velamen of Tripterygium wilfordii is used 30L 70% ethanol percolation 10 hours, collect percolate, concentrating under reduced pressure obtains ethanol extract, ethanol extract is with chloroform extraction 3 times, and the chloroform medicinal extract that concentrating under reduced pressure obtains is with 20% sulphuric acid extraction 6 times, filtering and collecting filter liquid, it is between the 8-11 that filtrate is regulated the pH value with sodium bicarbonate, separate out solid, filter back solid deionized water wash 6 times, obtain thick total alkaloids 32g behind the solid drying.
2, thick total alkaloids fully dissolves with 250mL methyl alcohol, filters and collects filter residue, and filter residue obtains pure total alkaloids 12g with the crystallization of methyl alcohol thermosol.
3, separate pure total alkaloids with high-speed counter-current chromatograph (TBE-1000A is produced with the biochemical company limited in field in Shanghai), the high performance liquid phase of pure total alkaloids detects color atlas as shown in Figure 7.
1) applied sample amount 700mg adopts normal hexane: ethyl acetate: ethanol: water=5: 5: 5: the solvent systems of 5 (v/v/v/v); Column volume 1000mL, rotating speed are 500rpm, 25 ℃ of column temperatures, below be stationary phase mutually, be moving phase mutually down, flow velocity 3mL/min, the stationary phase retention value of system is 69%, ultraviolet detection wavelength 254nm, detected result is seen accompanying drawing 2, a, b, c, d are respectively the adverse current chromatogram peak of wilfortrine, wilfordine, Wilforgine 20 and Wilforine.
2) operation steps is: at first place separating funnel by above-mentioned volume ratio preparation solvent systems, after shaking up, standing demix, isoequilibrium separated mutually with upper and lower after for some time.Then, use earlier as stationary phase, be full of whole pillar, adjust main frame and just change, rotating speed is 500rmp, will descend phase moving phase to pump in the post from the head end of pillar with the flow velocity of 3.0mL/min; After treating that whole system is set up running balance, go up the pure total alkaloids raw material of phased soln 700mg with 40mL, by the sampling valve sample introduction; Collect target compound according to the detector spectrogram then, obtain wilfortrine 90mg, wilfordine 100mg, Wilforgine 20 220mg, Wilforine 210mg respectively through recrystallizing methanol.High performance liquid phase check and analysis condition: chromatographic column is Zorbax SB C-18HPLC post (250mm * 4.6mm i.d, 5 μ m, Agilent), 35 ℃ of column temperatures, moving phase is acetonitrile: water=55: 45 (v/v), flow velocity 0.8mL/min, ultraviolet detection wavelength 254nm detect gained alkaloid monomer purity, the results are shown in accompanying drawing 3-6.
Embodiment 3:
1, the 10kg velamen of Tripterygium wilfordii is used 30L 80% ethanol percolation 10 hours, collect percolate, concentrating under reduced pressure obtains ethanol extract, ethanol extract is with chloroform extraction 3 times, and the chloroform medicinal extract that concentrating under reduced pressure obtains is with 20% acetic acid extraction 6 times, filtering and collecting filter liquid, it is between the 8-11 that filtrate is regulated the pH value with yellow soda ash, separate out solid, filter back solid deionized water wash 6 times, obtain thick total alkaloids 35g behind the solid drying.
2, thick total alkaloids fully dissolves with 250mL methyl alcohol, filters and collects filter residue, and filter residue obtains pure total alkaloids 14g with the crystallization of methyl alcohol thermosol.
3, separate pure total alkaloids with high-speed counter-current chromatograph (TBE-1000A is produced with the biochemical company limited in field in Shanghai), the high performance liquid phase of pure total alkaloids detects color atlas as shown in Figure 7.
1) applied sample amount 700mg adopts normal hexane: ethyl acetate: ethanol: water=6: 4: 5: the solvent systems of 8 (v/v/v/v); Column volume 1000mL, rotating speed are 500rpm, 25 ℃ of column temperatures, below be stationary phase mutually, be moving phase mutually down, flow velocity 5mL/min, the stationary phase retention value of system is 72%, ultraviolet detection wavelength 254nm, detected result is seen accompanying drawing 1, a, b, c, d are respectively the adverse current chromatogram peak of wilfortrine, wilfordine, Wilforgine 20 and Wilforine.
2) operation steps is: at first place separating funnel by above-mentioned volume ratio preparation solvent systems, after shaking up, standing demix, isoequilibrium separated mutually with upper and lower after for some time.Then, use earlier as stationary phase, be full of whole pillar, adjust main frame and just change, rotating speed is 500rmp, will descend phase moving phase to pump in the post from the head end of pillar with the flow velocity of 5.0mL/min; After treating that whole system is set up running balance, go up the pure total alkaloids raw material of phased soln 700mg with 40mL, by the sampling valve sample introduction; Collect target compound according to the detector spectrogram then, obtain wilfortrine 85mg, wilfordine 95mg, Wilforgine 20 215mg, Wilforine 200mg respectively through recrystallizing methanol.High performance liquid phase check and analysis condition: chromatographic column is Zorbax SB C-18HPLC post (250mm * 4.6mm i.d, 5 μ m, Agilent), 35 ℃ of column temperatures, moving phase is acetonitrile: water=55: 45 (v/v), flow velocity 0.8mL/min, ultraviolet detection wavelength 254nm detect gained alkaloid monomer purity, the results are shown in accompanying drawing 3-6.
Embodiment 4:
1, the 10kg velamen of Tripterygium wilfordii is used 30L 100% ethanol percolation 10 hours, collect percolate, concentrating under reduced pressure obtains ethanol extract, ethanol extract is with chloroform extraction 6 times, and the chloroform medicinal extract that concentrating under reduced pressure obtains is with 20% hydrochloric acid extraction 6 times, filtering and collecting filter liquid, it is between the 8-11 that filtrate is regulated the pH value with sodium hydroxide, separate out solid, filter back solid deionized water wash 3 times, obtain thick total alkaloids 38g behind the solid drying.
2, thick total alkaloids fully dissolves with 300mL methyl alcohol, filters and collects filter residue, and filter residue obtains pure total alkaloids 16g with the crystallization of methyl alcohol thermosol.
3, separate pure total alkaloids with high-speed counter-current chromatograph (TBE-1000A is produced with the biochemical company limited in field in Shanghai), the high performance liquid phase of pure total alkaloids detects color atlas as shown in Figure 7.
1) applied sample amount 700mg adopts normal hexane: ethyl acetate: ethanol: water=5: 5: 5: the solvent systems of 5 (v/v/v/v); Column volume 1000mL, rotating speed are 500rpm, 25 ℃ of column temperatures, below be stationary phase mutually, be moving phase mutually down, flow velocity 3mL/min, the stationary phase retention value of system is 69%, ultraviolet detection wavelength 254nm, detected result is seen accompanying drawing 2, a, b, c, d are respectively the adverse current chromatogram peak of wilfortrine, wilfordine, Wilforgine 20 and Wilforine.
2) operation steps is: at first place separating funnel by above-mentioned volume ratio preparation solvent systems, after shaking up, standing demix, isoequilibrium separated mutually with upper and lower after for some time.Then, use earlier as stationary phase, be full of whole pillar, adjust main frame and just change, rotating speed is 500rmp, will descend phase moving phase to pump in the post from the head end of pillar with the flow velocity of 3.0mL/min; After treating that whole system is set up running balance, go up the pure total alkaloids raw material of phased soln 700mg with 40mL, by the sampling valve sample introduction; Collect target compound according to the detector spectrogram then, obtain wilfortrine 90mg, wilfordine 100mg, Wilforgine 20 220mg, Wilforine 210mg respectively through recrystallizing methanol.High performance liquid phase check and analysis condition: chromatographic column is Zorbax SB C-18HPLC post (250mm * 4.6mm i.d, 5 μ m, Agilent), 35 ℃ of column temperatures, moving phase is acetonitrile: water=55: 45 (v/v), flow velocity 0.8mL/min, ultraviolet detection wavelength 254nm detect gained alkaloid monomer purity, the results are shown in accompanying drawing 3-6.
Claims (7)
1, a kind of counter current chromatography separates the method for preparing the trypterygine alkaloid monomer from trypterygine, it is characterized in that step is as follows:
1) trypterygine radical center, the dry pulverizing of root skin or stem, use ethanol percolation, the ethanolic soln extracting solution that diafiltration obtains is evaporated to the dried ethanol extract that obtains, ethanol extract chloroform extraction 3～6 times, obtain chloroform medicinal extract, chloroform medicinal extract is 8-11 with 3～6 after-filtration of acid extraction of mass percent concentration 4-20%, filtrate with alkali adjusting pH value, separates out solid, filter back deionized water wash 3～6 times, oven dry obtains thick total alkaloids, and thick total alkaloids is added the methyl alcohol mixing, filter, collect filter residue, drying obtains pure total alkaloids with recrystallizing methanol, is used for high speed adverse current chromatogram separation raw material;
3) with volume ratio be the alkane of 1-6: 1-7: 1-5: 1-8: fatty ester: Fatty Alcohol(C12-C14 and C12-C18): water preparation high speed adverse current chromatogram two-phase solvent system, place separating funnel, shake up, standing demix, after the balance, separate mutually upper and lower;
4) use the phase that fixes mutually, make moving phase mutually down, use the chromatogram pillar that is full of mutually in the whole counter current chromatograph, adjusting the counter current chromatograph main frame just changes, following phase moving phase pumped into from the head end of pillar carries out wash-out in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction; Perhaps with down as stationary phase, on make moving phase mutually, be full of whole adverse current chromatogram pillar mutually with following, the adjustment main frame is just changeing, and last phase moving phase is pumped into from the tail end of pillar carry out wash-out in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction; Spectrogram according to detector is collected target compound step by step, and concentrating under reduced pressure obtains each alkaloid monomer crude product, obtains wilfortrine, wilfordine, Wilforgine 20, Wilforine respectively through recrystallizing methanol again.
2, a kind of counter current chromatography according to claim 1 separates the method for preparing the trypterygine alkaloid monomer from trypterygine, and the volume ratio that it is characterized in that described ethanolic soln is 60-100%.
3, a kind of counter current chromatography according to claim 1 separates the method for preparing the trypterygine alkaloid monomer from trypterygine, it is characterized in that, described acid is hydrochloric acid, sulfuric acid or acetate.
4, a kind of counter current chromatography according to claim 1 separates the method for preparing the trypterygine alkaloid monomer from trypterygine, it is characterized in that, described alkali is sodium hydroxide, sodium bicarbonate or yellow soda ash.
5, a kind of counter current chromatography according to claim 1 separates the method for preparing the trypterygine alkaloid monomer from trypterygine, it is characterized in that, described alkane is normal hexane or sherwood oil, and described fatty ester is an ethyl acetate, and described Fatty Alcohol(C12-C14 and C12-C18) is an ethanol.
6, a kind of counter current chromatography according to claim 1 separates the method for preparing the trypterygine alkaloid monomer from trypterygine, it is characterized in that, described counter current chromatograph is the preparation type.
7, a kind of counter current chromatography according to claim 1 separates the method for preparing the trypterygine alkaloid monomer from trypterygine, it is characterized in that, described counter current chromatograph engine speed is 200-600rmp, and the flow velocity of described moving phase is 1.0-5.0mL/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101974005A (en) * | 2010-08-27 | 2011-02-16 | 浙江工商大学 | Preparation method of high-content sesquiterpenoids tripterygium alkaloid |
| CN102793737A (en) * | 2011-05-26 | 2012-11-28 | 澳门科技大学 | Method for preparing powder of effective part of thunder god vine |
| CN108191948A (en) * | 2018-02-06 | 2018-06-22 | 赖旭宇 | A kind of method for preparing triptolide and 2- table triptolides |
| CN110687224A (en) * | 2019-09-30 | 2020-01-14 | 浙江工业大学 | Method for measuring triptolide A in tripterygium wilfordii medicinal material and tripterygium wilfordii multi-glycoside tablet prepared from tripterygium wilfordii medicinal material |
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| CN1159308C (en) * | 1999-12-28 | 2004-07-28 | 杜琪珍 | Method for separating catechin monomer from tea extration |
| CN1136210C (en) * | 2000-08-07 | 2004-01-28 | 香港生物科技研究院有限公司 | High-speed countercurrent chromatographic process of separating and purifying tanshinol |
| CN1394870A (en) * | 2001-07-05 | 2003-02-05 | 北京天纯维通生物技术有限公司 | Method for separating and purifying tanshinone |
| CN1445223A (en) * | 2003-04-03 | 2003-10-01 | 浙江大学 | Method for preparing EGCG mono fatty acid ester by using high-speed countercurrent chromatographic separation |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974005A (en) * | 2010-08-27 | 2011-02-16 | 浙江工商大学 | Preparation method of high-content sesquiterpenoids tripterygium alkaloid |
| CN101974005B (en) * | 2010-08-27 | 2012-07-18 | 浙江工商大学 | Preparation method of high-content sesquiterpenoids tripterygium alkaloid |
| CN102793737A (en) * | 2011-05-26 | 2012-11-28 | 澳门科技大学 | Method for preparing powder of effective part of thunder god vine |
| CN108191948A (en) * | 2018-02-06 | 2018-06-22 | 赖旭宇 | A kind of method for preparing triptolide and 2- table triptolides |
| CN108191948B (en) * | 2018-02-06 | 2019-04-02 | 海门市彼维知识产权服务有限公司 | A method of preparing triptolide and 2- table triptolide |
| CN110687224A (en) * | 2019-09-30 | 2020-01-14 | 浙江工业大学 | Method for measuring triptolide A in tripterygium wilfordii medicinal material and tripterygium wilfordii multi-glycoside tablet prepared from tripterygium wilfordii medicinal material |
| CN110687224B (en) * | 2019-09-30 | 2022-04-19 | 浙江工业大学 | Method for measuring triptolide A in tripterygium wilfordii medicinal material and tripterygium wilfordii multi-glycoside tablet prepared from tripterygium wilfordii medicinal material |
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