CN1307170C - Method for separating effective ingredient lagehead atractylodes lactone III from lagehead atractylodes naphtha - Google Patents
Method for separating effective ingredient lagehead atractylodes lactone III from lagehead atractylodes naphtha Download PDFInfo
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- CN1307170C CN1307170C CNB2005100606436A CN200510060643A CN1307170C CN 1307170 C CN1307170 C CN 1307170C CN B2005100606436 A CNB2005100606436 A CN B2005100606436A CN 200510060643 A CN200510060643 A CN 200510060643A CN 1307170 C CN1307170 C CN 1307170C
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Abstract
The present invention discloses a method for separating effective ingredient lagehead atractylodes lactone III from lagehead atractylodes volatile oil. Comminuted lagehead atractylodes powder is leached with medium polar solvent, the solvent is recovered, and russet volatile oil is obtained. Alcohol with low carbon chain is used for dissolving volatile oil and is placed at the temperature of -4 DEG C to 0 DEG C, insoluble substance is removed, filter liquor is concentrated, and refined volatile oil can be obtained. The volatile oil is dissolved with the medium polar solvent, low polar solvent is gradually added until the concentration of the low polar solvent reaches from 80% to 90%, and precipitates are eliminated. The filter liquor is concentrated and is degreased with the low polar solvent to carry out recrystallization, and colorless needle crystal lagehead atractylodes lactone III can be obtained. The present invention has simple process, the cost of the obtained lagehead atractylodes lactone III is low, and the purity is high.
Description
Technical field
The invention belongs to the Chinese medicine pharmaceutical field, relate in particular to a kind of from Rhizoma Atractylodis Macrocephalae volatile oil the method for separating effective ingredient atractylenolide II.
Background technology
The bighead atractylodes rhizome is a kind of traditional Chinese medicinal materials, is the dry rhizome of the feverfew bighead atractylodes rhizome (Atractylodes macrocephalaKoidz.).The bighead atractylodes rhizome is called in art, winter art, Zhejiang art etc., is per nnial herb.It is warm in nature, and it is sweet, bitter to distinguish the flavor of.Invigorating the spleen and benefiting QI, eliminating dampness Li Shui, hidroschesis, antiabortive function are arranged.Be mainly used in insufficiency of the spleen food less, maldigestion, abdominal distension have loose bowels, lassitude, phlegm and retained fluid are dizzyly throbbed with fear, oedema, spontaneous perspiration, threatened abortion, is Chinese medicine tonifying spleen key medicine.Modern pharmacological research shows, effect such as the bighead atractylodes rhizome protects the liver, cholagogic, diuresis, antibacterial, anti-inflammatory, antitumor, strengthening immunity, step-down, hypoglycemic, anticoagulation, strong, calmness.
The chemical ingredients of the bighead atractylodes rhizome is mainly Rhizoma Atractylodis Macrocephalae volatile oil, oily displaing yellow, and thickness has fragrance.Main effective constituent is atractylone in the bighead atractylodes rhizome, atractylodes lactone class and soluble polysaccharide.Atractylenolide, II, III are effective content of anti inflammation (Endo, K., Toguchi, T., Toguchi, F., Hikino, H., Yamahara, J.and Fujimura, H., 1979:Antiinflammatory and autoxidation ofatractylone.Chem.Pharm.Bull., 12:755-760), Rhizoma Atractylodis Macrocephalae volatile oil and atractylenolide II have antitumous effect (Tang Defang, Hao Yuhang, Liu Zuoya, the seedling woods, Wei Hua, sky is strong, Pingjiang River bighead atractylodes rhizome rhizome volatile oil component and tumor-inhibiting action research thereof, pharmacy circular, 1984,19 (9): 43-46).
Atractylenolide II (atractylenoide III) belongs to sesquiterpene lactones class chemicals, and molecular formula is C
15H
20O
3, molecular structural formula is:
Atractylenolide II is colourless needle, is dissolved in methyl alcohol, ethanol, ethyl acetate etc., is insoluble to low polar solvents such as sherwood oil, normal hexane.
Atractylenolide II content in the bighead atractylodes rhizome is very low, accounts for 0.01-0.05% (bighead atractylodes rhizome), because atractylone instability in the volatile oil, very easily oxidation generates atractylodes lactone class material.Therefore, in the Rhizoma Atractylodis Macrocephalae (parched) content of atractylenolide II apparently higher than Rhizoma Atractylodis Macrocephalae.The content of atractylenolide II is low, makes its separation difficulty.The method of separation atractylenolide II commonly used is that column chromatography is separated in the document, and this separation method is wasted time and energy, and the industrialization difficulty.
Summary of the invention
The object of the invention provide a kind of simple, cost is low, simple to operate, be fit to industrial from Rhizoma Atractylodis Macrocephalae volatile oil the method for separating effective ingredient atractylenolide II.
A kind of from Rhizoma Atractylodis Macrocephalae volatile oil the step of the method for separating effective ingredient atractylenolide II as follows:
1) uses the solvent of middle polarity to leach in the bighead atractylodes rhizome powder of pulverizing, reclaim solvent and get tawny volatile oil;
2) dissolve volatile oil and place-4 ℃～0 ℃ with low carbon chain alcohol, remove insolubles, concentrating filter liquor obtains purified volatile oil;
3) volatile oil dissolves with medium polar solvent, progressively adds low polar solvent then, reaches volume percent 80～90%, disgorging up to low polar solvent concentration;
4) filtrate is concentrated and, can obtain the atractylenolide II of colourless needle crystal with carrying out recrystallization after the low polar solvent degreasing.
Another kind step of the method for separating effective ingredient atractylenolide II from Rhizoma Atractylodis Macrocephalae volatile oil is as follows:
1) with the bighead atractylodes rhizome powder low polar solvent degreasing of pulverizing;
2) bighead atractylodes rhizome after the degreasing leaches with medium polar solvent, reclaims solvent and gets tawny volatile oil;
3) volatile oil dissolves with medium polar solvent, progressively adds low polar solvent then, reaches volume percent 80～90%, disgorging up to low polar solvent concentration;
4) filtrate is concentrated and, can obtain the atractylenolide II of colourless needle crystal with carrying out recrystallization after the low polar solvent degreasing.
Described low polar solvent is sherwood oil, normal hexane, hexanaphthene, normal heptane or their mixture; Medium polar solvent is methylene dichloride, trichloromethane, tetracol phenixin, ethylene dichloride, ethyl acetate or their mixture; Low carbon chain alcohol is methyl alcohol, ethanol, propyl alcohol or their mixture.Solvent leaching or solvent degreasing be adopt that cold soaking, heat are carried, Soxhlet extraction, diacolation or ultrasonically auxiliary extracting method, described solvent recuperation and filtrate concentrating adopted air distillation or underpressure distillation.Recrystallization solvent is the mixture with rudimentary property solvent and medium polar solvent, and the blended volume ratio is 8: 1～10: 1.
Advantage of the present invention is: the bighead atractylodes rhizome is a kind of herbal medicine commonly used, and the column chromatography methods that adopt feasible in the column chromatography methods laboratory more in the separation document of its effective constituent, but be difficult for realizing for a large amount of preparations.The present invention is simple to operate, and is convenient.
Description of drawings
Accompanying drawing is the schema of separating effective ingredient atractylenolide II from Rhizoma Atractylodis Macrocephalae volatile oil.
Embodiment
Embodiment 1:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder,, reclaim solvent and get tawny volatile oil with the ethyl acetate leaching 3 times (each 1h, 70 ℃ of waters bath with thermostatic control, mixing speed 500r/min) of 6 times of volumes.With dissolve with methanol volatile oil and place 0 ℃ 24 hours, remove insolubles, filtrate decompression distillation obtains purified volatile oil.Volatile oil progressively adds sherwood oil (60～90 ℃) then with the acetic acid ethyl dissolution of 2 times of volumes, reaches 80% up to final volume concentration, removes precipitation.Filtrate decompression distillation concentrated and with sherwood oil (60～90 ℃) degreasing of 8 times of volumes 4 times (1h at every turn, 60 ℃ of waters bath with thermostatic control, mixing speed 300r/min), carry out recrystallization (sherwood oil-ethyl acetate volume ratio 10: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.0% (in the volatile oil) of yield.
Embodiment 2:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dry under 60 ℃ in baking oven, pulverize, get bighead atractylodes rhizome powder, with the methylene dichloride room temperature leaching 3 times (each 1h, mixing speed 400r/min) of 8 times of volumes, the recovery solvent gets tawny volatile oil.With anhydrous alcohol solution volatile oil and place-4 ℃ 24 hours, remove insolubles, the filtrate air distillation obtains purified volatile oil.Volatile oil progressively adds normal hexane then with the methylene dichloride dissolving of 2 times of volumes, reaches 90% up to final volume concentration, removes precipitation.Filtrate decompression distillation concentrated and with the normal hexane room temperature leaching degreasing of 4 times of volumes 3 times (1h at every turn, 500r/min), carry out recrystallization (normal hexane-methylene chloride volume was than 9: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.6% (in the volatile oil) of yield.
Embodiment 3:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder, extracts (3h at every turn) 2 times with the trichloromethane of 8 times of volumes in the Soxhlet extraction element, the recovery solvent gets tawny volatile oil.With propyl alcohol dissolving volatile oil and place-2 ℃ 24 hours, remove insolubles, filtrate concentrates through underpressure distillation and obtains purified volatile oil.Volatile oil progressively adds hexanaphthene then with the trichloromethane dissolving of 2 times of volumes, reaches 85% up to final volume concentration, removes precipitation.The filtrate air distillation concentrated and with the hexanaphthene degreasing of 6 times of volumes 3 times (1h at every turn, 60 ℃ of waters bath with thermostatic control, mixing speed 300r/min), carry out recrystallization (hexanaphthene-trichloromethane volume ratio 10: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.2% (in the volatile oil) of yield.
Embodiment 4:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder, in the diacolation device, extract 2 times, reclaim solvent and get tawny volatile oil with tetracol phenixin.With anhydrous alcohol solution volatile oil and place-3 ℃ 24 hours, remove insolubles, filtrate concentrates through underpressure distillation and obtains purified volatile oil.Volatile oil progressively adds suberane then with the tetracol phenixin dissolving of 2 times of volumes, reaches 90% up to final volume concentration, removes precipitation.Filtrate decompression concentrated and with the suberane degreasing of 6 times of volumes 3 times (1h at every turn, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min), carry out recrystallization (suberane-tetracol phenixin volume ratio 9: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.4% (in the volatile oil) of yield.
Embodiment 5:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder, with the tetracol phenixin and the trichloromethane (volume ratio 1: 1) of 8 times of volumes, extract (each 1h, room temperature in the ultrasonic assisted extraction device 3 times, mixing speed 300r/min), reclaim solvent and get tawny volatile oil.With anhydrous methanol and dehydrated alcohol (volume ratio 1: 1) dissolving volatile oil and place-4 ℃ 24 hours, remove insolubles, filtrate concentrates through underpressure distillation and obtains purified volatile oil.Volatile oil progressively adds normal hexane then with the acetic acid ethyl dissolution of 2 times of volumes, reaches 80% up to final volume concentration, removes precipitation.Filtrate decompression distillation concentrated and with 6 times of amount normal hexanes and sherwood oil (60-90 ℃) (volume ratio 1: 1) degreasing 3 times (1h at every turn, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min), carry out recrystallization (normal hexane-ethyl acetate volume ratio 8: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.5% (in the volatile oil) of yield.
Embodiment 6:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder, in the diacolation device, extract 2 times, slough fat-soluble component with sherwood oil (60～90 ℃).The bighead atractylodes rhizome after the degreasing leaches (each 1h, 70 ℃ of waters bath with thermostatic control, mixing speed 500r/min) 3 times with the ethyl acetate of 8 times of volumes.Underpressure distillation concentrates the recovery ethyl acetate and gets tawny volatile oil.Volatile oil progressively adds sherwood oil (60～90 ℃) then with the acetic acid ethyl dissolution of 2 times of volumes, reaches 90% up to final volume concentration, removes precipitation.Filtrate decompression concentrated and with 6 times of amount sherwood oils (60～90 ℃) degreasing 3 times (1h at every turn, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min), carry out recrystallization (sherwood oil-ethyl acetate volume ratio 8: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.7% (in the volatile oil) of yield.
Embodiment 7:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dry under 60 ℃ in baking oven, pulverize, get bighead atractylodes rhizome powder, with normal hexane degreasing 2 times (each 3h) in the Soxhlet extraction element of 6 times of volumes.The bighead atractylodes rhizome after the degreasing extracts (each 3h) 2 times with the methylene dichloride of 6 times of volumes in the Soxhlet extraction element.Underpressure distillation concentrates the recovery methylene dichloride and gets tawny volatile oil.Volatile oil progressively adds normal hexane then with the methylene dichloride dissolving of 2 times of volumes, reaches 90% up to final volume concentration, removes precipitation.Filtrate decompression distillation concentrated and with the normal hexane degreasing of 6 times of volumes 3 times (1h at every turn, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min), carry out recrystallization (normal hexane-methylene chloride volume was than 10: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 3.2% (in the volatile oil) of yield.
Embodiment 8:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder, with hexanaphthene degreasing 3 times (each 1h, room temperature, mixing speed 300r/min) in ultrasonic assisted extraction device of 6 times of volumes.The bighead atractylodes rhizome after the degreasing is with the trichloromethane room temperature of 6 times of volumes leaching 3 times (each 1h,, mixing speed 500r/min).Underpressure distillation concentrates the recovery trichloromethane and gets tawny volatile oil.Volatile oil progressively adds hexanaphthene then with the trichloromethane dissolving of 2 times of volumes, reaches 80% up to final volume concentration, removes precipitation.Filtrate concentrated and with the hexanaphthene degreasing of 6 times of volumes 3 times (1h at every turn, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min), carry out recrystallization (hexanaphthene-trichloromethane volume ratio 9: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.3% (in the volatile oil) of yield.
Embodiment 9:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder, with the suberane degreasing 3 times (each 1h, 70 ℃ of waters bath with thermostatic control, mixing speed 500r/min) of 6 times of volumes.The bighead atractylodes rhizome after the degreasing leaches (each 1h, mixing speed 500r/min) 3 times with the tetracol phenixin room temperature of 6 times of volumes.Underpressure distillation concentrates the recovery tetracol phenixin and gets tawny volatile oil.Volatile oil progressively adds suberane then with the tetracol phenixin dissolving of 2 times of volumes, reaches 90% up to final volume concentration, removes precipitation.Filtrate concentrated and with the suberane degreasing of 6 times of volumes 3 times (1h at every turn, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min), carry out recrystallization (suberane-tetracol phenixin volume ratio 10: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 2.9% (in the volatile oil) of yield.
Embodiment 10:
The bighead atractylodes rhizome (Xinchang, Zhejiang) is dried naturally, pulverize, get bighead atractylodes rhizome powder, with the mixture degreasing of the normal hexane of 6 times of volumes and hexanaphthene (volume ratio 1: 1) 3 times (1h, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min) at every turn.The bighead atractylodes rhizome after the degreasing leaches (each 1h, 60 ℃ of waters bath with thermostatic control, mixing speed 500r/min) 3 times with the ethyl acetate of 6 times of volumes.Underpressure distillation concentrates the recovery ethyl acetate and gets tawny volatile oil.Volatile oil progressively adds normal hexane then with the tetracol phenixin dissolving of 2 times of volumes, reaches 80% up to final volume concentration, removes precipitation.Filtrate decompression concentrated and with the normal hexane of 6 times of volumes and sherwood oil (60～90 ℃) (volume ratio 1: 1) degreasing 3 times (1h at every turn, 50 ℃ of waters bath with thermostatic control, mixing speed 500r/min), carry out recrystallization (normal hexane-ethyl acetate volume ratio 8: 1), can obtain the atractylenolide II of colourless needle crystal, purity＞95%, about 3.1% (in the volatile oil) of yield.
Differentiate
Gas-chromatography-mass spectrometry combination method (GC-MS):
The atractylenolide II crystal that takes a morsel carries out GC-MS and analyzes, instrument: TRACEGC2000/TRACE MS (the thermoelectric instrument company of ThermoQuest) .GC condition: chromatographic column HP-530m * 0.25mm * 0.25 μ m, 50 ℃ of (2min)-15 of column temperature ℃/min-240 ℃ (10min), 260 ℃ of sample introduction temperature, splitting ratio 10: 1, sample size 1 μ l.Carrier gas: He, flow velocity 1ml/min, EIMS condition: electron energy 70Ev, mass range 35～500,200 ℃ of ion source temperatures, 250 ℃ of interface temperatures.The retention time of atractylenolide II is 14.00min.
Infrared spectra:
Atractylenolide II crystal is measured with pellet technique (Impact-410, U.S. Nicolet company) on infrared spectrometer.
Nuclear magnetic resonance spectrum:
With atractylenolide II crystal do hydrogen (
1H) nuclear magnetic resonance spectroscopy.Instrument: Advance DMX500 Switzerland Bruker company, operating frequency:
1H-NMR 500MHz, solvent: deuterochloroform (CDCl
3).
With the MS of this compound, IR,
1The H-NMR spectrum contrasts with document, is accredited as atractylenolide II.
The comprehensive above susceptible of proof of analyzing, the present invention separates the colourless acicular crystal that obtains from Rhizoma Atractylodis Macrocephalae volatile oil be atractylenolide II.
Claims (6)
1. the method for a separating effective ingredient atractylenolide II from Rhizoma Atractylodis Macrocephalae volatile oil is characterized in that the step of method is as follows:
1) uses the solvent of middle polarity to leach in the bighead atractylodes rhizome powder of pulverizing, reclaim solvent and get tawny volatile oil;
2) dissolve volatile oil and place-4 ℃～0 ℃ with low carbon chain alcohol, remove insolubles, concentrating filter liquor obtains purified volatile oil;
3) volatile oil dissolves with medium polar solvent, progressively adds low polar solvent then, reaches volume percent 80～90%, disgorging up to low polar solvent concentration;
4) filtrate is concentrated and, can obtain the atractylenolide II of colourless needle crystal with carrying out recrystallization after the low polar solvent degreasing;
Described low polar solvent is sherwood oil, normal hexane, hexanaphthene, normal heptane or their mixture; Medium polar solvent is methylene dichloride, trichloromethane, tetracol phenixin, ethylene dichloride, ethyl acetate or their mixture; Low carbon chain alcohol is methyl alcohol, ethanol, propyl alcohol or their mixture.
2. according to claim 1 a kind of from Rhizoma Atractylodis Macrocephalae volatile oil the method for separating effective ingredient atractylenolide II, it is characterized in that: leaching of described solvent or solvent degreasing be adopt that cold soaking, heat are carried, Soxhlet extraction, diacolation or ultrasonically auxiliary extracting method, described solvent recuperation and filtrate concentrating adopted air distillation or underpressure distillation.
3. according to claim 1 a kind of from Rhizoma Atractylodis Macrocephalae volatile oil the method for separating effective ingredient atractylenolide II, it is characterized in that: described recrystallization solvent is the mixture with rudimentary property solvent and medium polar solvent, and the blended volume ratio is 8: 1～10: 1.
4. the method for a separating effective ingredient atractylenolide II from Rhizoma Atractylodis Macrocephalae volatile oil is characterized in that the step of method is as follows:
1) with the bighead atractylodes rhizome powder low polar solvent degreasing of pulverizing;
2) bighead atractylodes rhizome after the degreasing leaches with medium polar solvent, reclaims solvent and gets tawny volatile oil;
3) volatile oil dissolves with medium polar solvent, progressively adds low polar solvent then, reaches volume percent 80～90%, disgorging up to low polar solvent concentration;
4) filtrate is concentrated and, can obtain the atractylenolide II of colourless needle crystal with carrying out recrystallization after the low polar solvent degreasing;
Described low polar solvent is sherwood oil, normal hexane, hexanaphthene, normal heptane or their mixture; Medium polar solvent is methylene dichloride, trichloromethane, tetracol phenixin, ethylene dichloride, ethyl acetate or their mixture; Low carbon chain alcohol is methyl alcohol, ethanol, propyl alcohol or their mixture.
5. according to claim 4 a kind of from Rhizoma Atractylodis Macrocephalae volatile oil the method for separating effective ingredient atractylenolide II, it is characterized in that: leaching of described solvent or solvent degreasing adopt that cold soaking, heat are carried, Soxhlet extraction, diacolation or ultrasonically auxiliary extracting method, and described solvent recuperation and filtrate concentrating adopted air distillation or underpressure distillation.
6. according to claim 4 a kind of from Rhizoma Atractylodis Macrocephalae volatile oil the method for separating effective ingredient atractylenolide II, it is characterized in that: described recrystallization is the mixture with low polar solvent and medium polar solvent, the blended volume ratio is 8: 1～10: 1.
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| CN106074652A (en) * | 2016-07-11 | 2016-11-09 | 周晗生 | The extracting method of Rhizoma Atractylodis Macrocephalae extract |
| CN107674053B (en) * | 2017-10-23 | 2019-08-20 | 北京恒生佳合细胞科技有限公司 | A kind of atractylodes lactone V, preparation method and the application of aspect is frozen in CIK cell |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09241159A (en) * | 1996-03-06 | 1997-09-16 | Kureha Chem Ind Co Ltd | Synthesis suppressant containing atractylenolide iii for protein belonging to hsp60 family |
| JPH1045585A (en) * | 1996-07-31 | 1998-02-17 | Kureha Chem Ind Co Ltd | Synthetic inhibitor containing atractylenolide iii of protein belonging to hsp 27 family |
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2005
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09241159A (en) * | 1996-03-06 | 1997-09-16 | Kureha Chem Ind Co Ltd | Synthesis suppressant containing atractylenolide iii for protein belonging to hsp60 family |
| JPH1045585A (en) * | 1996-07-31 | 1998-02-17 | Kureha Chem Ind Co Ltd | Synthetic inhibitor containing atractylenolide iii of protein belonging to hsp 27 family |
Non-Patent Citations (5)
| Title |
|---|
| 中草药 王惠康等，195.197，党参的化学成分研究 1991 * |
| 关苍术极性化学成分的分离及结构鉴定 金玉兰等，37.38，关苍术极性化学成分的分离及结构鉴定 1992 * |
| 关苍术极性化学成分的分离及结构鉴定 金玉兰等，37.38，关苍术极性化学成分的分离及结构鉴定 1992;山东医药工业 董岩等，32.33，白术化学成分研究新进展 2003;植物学把 黄宝山等，614.617，白术内酯IV的分离鉴定 1992;中草药 王惠康等，195.197，党参的化学成分研究 1991 * |
| 山东医药工业 董岩等，32.33，白术化学成分研究新进展 2003 * |
| 植物学把 黄宝山等，614.617，白术内酯IV的分离鉴定 1992 * |
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