CN102219823A - Method for extracting shionone from aster tataricus - Google Patents
Method for extracting shionone from aster tataricus Download PDFInfo
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- CN102219823A CN102219823A CN2011101516803A CN201110151680A CN102219823A CN 102219823 A CN102219823 A CN 102219823A CN 2011101516803 A CN2011101516803 A CN 2011101516803A CN 201110151680 A CN201110151680 A CN 201110151680A CN 102219823 A CN102219823 A CN 102219823A
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Abstract
The invention discloses a method for extracting shionone from aster tataricus. The method is characterized by comprising the steps of crushing aster tataricus, adding 5-7 times of 80-90 percent methanol for backflow extraction for 2-3 times, adding active carbon into the extract for decoloring, filtering with heat, concentrating 30-50 percent alcohol for crystallization, filtering out crystal and dissolving the crystal with alkaline alcohol solution, filtering and adjusting pH to 2-5 for standing and precipitating, filtering out precipitate and dissolving with alkaline alcohol solution, filtering and adjusting to be neutral for precipitation, filtering out alcohol for backflow and dissolving for recrystallization for 2-3 times, and drying, thus obtaining shionone. In the method, the process operation is simple, the obtained product content is high and industrial production is easy.
Description
Technical field:
The invention belongs to the natural drug separation field, especially relate to a kind of method of from aster, extracting Shionone.
Background technology:
Aster has another name called aster, short braid, clamping plate dish, donkey ear dish, soft aster, is a kind of common feverfew, is the root and rhizome of feverfew aster Aster tataricus L.f..Traditional medicine thinks that it is warm in nature, bitter, suffering, and moistening lung to lower QI has the effect of stopping coughing and removing phlegm, is usually used in being used for the treatment of the disease that phlegm is breathed with cough more, newly chronic cough is coughed, labor is coughed hemoptysis.Modern medicine study shows that the aster medicinal material contains Shionone (shionone), Quercetin, friedelin, epi-friedelin and volatilization wet goods composition.Liu can wait in activity experiment the proof Shionone can significantly suppress mouse cough due to the ammoniacal liquor more.Chinese Pharmacopoeia regulation Shionone is the index composition.
Shionone chemical name 2-shinonen-3-one, molecular formula C
30H
50O, molecular weight 426.7, molecular structure is:
Shionone is a colourless crystallization, can be dissolved in organic solvents such as sherwood oil, benzene, ether, chloroform, and is water insoluble.Aceticanhydride-strong sulfuric acid response is positive, and the Tricholroacetic Acid reaction is positive fusing point 161-162 ℃.
Extract Shionone technology from the aster medicinal material, disclose lessly, be mostly employing 90-95% extraction using alcohol, concentrated solution petroleum ether extraction, silicagel column separate repeatedly and obtain Shionone." HPLC-ELSD of the isolation identification of effective constituent and the Shionone mensuration in the aster " that waits " chemical constitution study of aster " deliver and Zhang Bin etc. to deliver as Jin Jing.Adopt supercritical CO in addition in addition
2Extraction process, wait " the supercritical CO of delivering as Shangzhi not
2The technical study of Shionone in the extraction aster " can obtain the Shionone of content 80%.Though this kind method is simple, cleanliness without any pollution, equipment one-time investment height, extracted amount is less, also is not suitable for suitability for industrialized production.
Summary of the invention:
The objective of the invention is to overcome the defective of prior art, a kind of method of extracting Shionone from aster is provided, technology is simple, is easy to suitability for industrialized production.
The objective of the invention is to be achieved through the following technical solutions:
Get the aster pulverizing medicinal materials, add 5-7 and doubly measure 80-90% methanol eddy extraction 2-3 time, extracting solution adds activated carbon decolorizing, filtered while hot, be concentrated into determining alcohol 30-50% and place crystallization, crystallisate leaches with the alkaline alcohol solution dissolving, filters to regulate pH2-5 placement precipitation, leaches throw out and dissolves with alkaline alcohol solution, filtration is adjusted to neutrality, staticly settle, leach alcohol reflux dissolving-recrystallization 2-3 time, be drying to obtain.
Described gac is a medicinal carbon, and consumption is the 1-3% of amount of liquid.
Described alkaline alcohol is: optional sodium hydroxide of alkali or potassium hydroxide, alcohol is methyl alcohol or the ethanolic soln of concentration 75-85%, mass ratio 1: 100-200.
The 7-10 that described alkaline alcohol consumption is a solute doubly measures.
A kind of in the optional hydrochloric acid of described acid, sulfuric acid, phosphoric acid or the acetic acid.
Advantage of the present invention is: the method for process using hydrotropy increases Shionone solubleness in low-carbon alcohol, remove impurity, overcome prior art and adopted of the harm of volatile toxic reagents such as sherwood oil, chloroform environment and operator, also solved simultaneously the defective of silicagel column separation industries difficulty, whole process flow is simple, has realized the suitability for industrialized production of Shionone.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get the aster pulverizing medicinal materials, weighing 10kg, drop into the pilot scale extractor, add 50kg 80% methanol eddy and extracted 2 hours, leach liquid, add equal-volume solution refluxing extraction 1 hour again, united extraction liquid added 2kg medical active carbon decoloring 2 hours, after leaching gac while hot, be concentrated into determining alcohol 50% and place crystallization 12 hours, filter the 105g crystallisate.Get the dissolving crystallized thing of 800ml75% ethanolic soln (containing 4g sodium hydroxide), filter, hydrochloric acid is placed precipitation after regulating pH2, leaches throw out 500ml75% ethanolic soln (containing 2.5g sodium hydroxide) dissolving again, filters, hydrochloric acid is adjusted to neutrality, staticly settle, leach throw out, be drying to obtain Shionone crystal 11.5g with 90% alcohol reflux dissolving-recrystallization 3 times, detect content 95.1% through HPLC.
Embodiment 2:
Get the aster pulverizing medicinal materials, weighing 10kg drops into the pilot scale extractor, add 50kg 90% methanol eddy and extracted 1 hour, extract 3 times, united extraction liquid added 3kg medical active carbon decoloring 2 hours, after leaching gac while hot, be concentrated into determining alcohol 30% and place crystallization 15 hours, filter the 116g crystallisate.Get the dissolving crystallized thing of 1000ml85% ethanolic soln (containing 6g potassium hydroxide), filter, sulfuric acid is placed precipitation after regulating pH5, leaches throw out 800ml85% ethanolic soln (containing 4g potassium hydroxide) dissolving again, filters, sulfuric acid is adjusted to neutrality, staticly settle, leach throw out, be drying to obtain Shionone crystal 9.5g with 95% alcohol reflux dissolving-recrystallization 3 times, detect content 98.1% through HPLC.
Embodiment 3:
Get the aster pulverizing medicinal materials, weighing 10kg, drop into the pilot scale extractor, add the 70kg90% methanol eddy and extracted 2 hours, leach liquid, add equal-volume solution refluxing extraction 1 hour again, united extraction liquid added 3kg medical active carbon decoloring 2 hours, after leaching gac while hot, be concentrated into determining alcohol 50% and place crystallization 9 hours, filter the 97g crystallisate.Get the dissolving crystallized thing of 800ml80% ethanolic soln (containing 4g sodium hydroxide), filter, phosphoric acid is placed precipitation after regulating pH4, leaches throw out 800ml80% ethanolic soln (containing 4g sodium hydroxide) dissolving, filters, phosphoric acid is adjusted to neutrality, staticly settle, leach throw out, be drying to obtain Shionone crystal 8.5g with 90% alcohol reflux dissolving-recrystallization 3 times, detect content 98.3% through HPLC.
Embodiment 4:
Get the aster pulverizing medicinal materials, weighing 20kg, drop into the pilot scale extractor, add the 140kg80% methanol eddy and extracted 2 hours, leach liquid, add equal-volume solution refluxing extraction 1 hour again, united extraction liquid added 5kg medical active carbon decoloring 2 hours, after leaching gac while hot, be concentrated into determining alcohol 50% and place crystallization 8 hours, filter the 183g crystallisate.Get the dissolving crystallized thing of 1800ml85% ethanolic soln (containing 8g sodium hydroxide), filter, hydrochloric acid is placed precipitation after regulating pH5, leach throw out 1500ml85% ethanolic soln (containing 7g sodium hydroxide) dissolving again, filter hydrochloric acid and be adjusted to neutrality, staticly settle, leach throw out with 95% alcohol reflux dissolving-recrystallization 3 times, be drying to obtain Shionone crystal 19.9g, detect content 97.9% through HPLC.
Embodiment 5:
Get the aster pulverizing medicinal materials, weighing 50kg, drop into the pilot scale extractor, add 350kg 80% methanol eddy and extracted 2 hours, leach liquid, add equal-volume solution refluxing extraction 1 hour again, united extraction liquid added 15kg medical active carbon decoloring 2 hours, after leaching gac while hot, be concentrated into determining alcohol 50% and place crystallization 12 hours, filter the 498g crystallisate.Get the dissolving crystallized thing of 4L80% ethanolic soln (containing 20g sodium hydroxide), filter, sulfuric acid is placed precipitation after regulating pH5, leach throw out 4L80% ethanolic soln (containing 20g sodium hydroxide) dissolving, filter hydrochloric acid and be adjusted to neutrality, staticly settle, leach throw out with 90% alcohol reflux dissolving-recrystallization 3 times, be drying to obtain Shionone crystal 5 1.5g, detect content 98.4% through HPLC.
Claims (5)
1. a method of extracting Shionone from aster is characterized in that: get the aster pulverizing medicinal materials, add 5-7 and doubly measure 80-90% methanol eddy extraction 2-3 time, extracting solution adds activated carbon decolorizing, filtered while hot is concentrated into determining alcohol 30-50% and places crystallization, and crystallisate leaches with alkaline alcohol solution and dissolves, place precipitation after filtering adjusting pH2-5, leach throw out again with the alkaline alcohol solution dissolving, filter and be adjusted to neutrality, staticly settle, leach alcohol reflux dissolving-recrystallization 2-3 time, be drying to obtain.
2. extract the method for Shionone according to claim 1 from aster, it is characterized in that described gac is a medicinal carbon, consumption is the 1-3% of amount of liquid.
3. extract the method for Shionone according to claim 1 from aster, it is characterized in that described alkaline alcohol is: optional sodium hydroxide of alkali or potassium hydroxide, alcohol is methyl alcohol or the ethanolic soln of concentration 75-85%, mass ratio 1: 100-200.
4. from aster, extract the method for Shionone according to claim 1, it is characterized in that the 7-10 that described alkaline alcohol consumption is a solute doubly measures.
5. from aster, extract the method for Shionone according to claim 1, it is characterized in that a kind of in the optional hydrochloric acid of described acid, sulfuric acid, phosphoric acid or the acetic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101516803A CN102219823A (en) | 2011-06-07 | 2011-06-07 | Method for extracting shionone from aster tataricus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101516803A CN102219823A (en) | 2011-06-07 | 2011-06-07 | Method for extracting shionone from aster tataricus |
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| CN102219823A true CN102219823A (en) | 2011-10-19 |
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| CN2011101516803A Pending CN102219823A (en) | 2011-06-07 | 2011-06-07 | Method for extracting shionone from aster tataricus |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669822A (en) * | 2016-02-02 | 2016-06-15 | 南京正亮医药科技有限公司 | Application of Epishionol to preparing of medicine for treating breast cancer |
| CN106916197A (en) * | 2017-04-28 | 2017-07-04 | 南宁馨艺荣生物科技有限公司 | Process for extracting shionone from beautiful millettia root |
| CN107383148A (en) * | 2017-06-30 | 2017-11-24 | 广西南宁桂知科技有限公司 | Purification shionon technique is extracted from beautiful millettia root |
| CN114767691A (en) * | 2022-04-15 | 2022-07-22 | 南京鼓楼医院 | Application of shionone in preparation of medicine for treating cerebral arterial thrombosis |
-
2011
- 2011-06-07 CN CN2011101516803A patent/CN102219823A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669822A (en) * | 2016-02-02 | 2016-06-15 | 南京正亮医药科技有限公司 | Application of Epishionol to preparing of medicine for treating breast cancer |
| CN106916197A (en) * | 2017-04-28 | 2017-07-04 | 南宁馨艺荣生物科技有限公司 | Process for extracting shionone from beautiful millettia root |
| CN107383148A (en) * | 2017-06-30 | 2017-11-24 | 广西南宁桂知科技有限公司 | Purification shionon technique is extracted from beautiful millettia root |
| CN114767691A (en) * | 2022-04-15 | 2022-07-22 | 南京鼓楼医院 | Application of shionone in preparation of medicine for treating cerebral arterial thrombosis |
| CN114767691B (en) * | 2022-04-15 | 2023-05-19 | 南京鼓楼医院 | Application of asterone in preparing medicine for treating ischemic cerebral apoplexy |
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Application publication date: 20111019 |