CN1450061A - Process for extracting Isofraxidin - Google Patents

Process for extracting Isofraxidin Download PDF

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Publication number
CN1450061A
CN1450061A CN02109476A CN02109476A CN1450061A CN 1450061 A CN1450061 A CN 1450061A CN 02109476 A CN02109476 A CN 02109476A CN 02109476 A CN02109476 A CN 02109476A CN 1450061 A CN1450061 A CN 1450061A
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China
Prior art keywords
isofraxidin
temperature
extraction
extracting method
extracting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN02109476A
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Chinese (zh)
Inventor
祖元刚
李庆勇
付玉杰
张宝友
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Northeast Forestry University
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Northeast Forestry University
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Publication date
Application filed by Northeast Forestry University filed Critical Northeast Forestry University
Priority to CN02109476A priority Critical patent/CN1450061A/en
Publication of CN1450061A publication Critical patent/CN1450061A/en
Pending legal-status Critical Current

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Abstract

The method for extracting isoforaxidin includes the following main processes: pulverizing root and rhizome of acanthopanax senticosus, drying, supercritical CO2 extraction, first separation, second separation, concentrating extract and vacuum drying so as to obtain the invented product. Said invention is high in extraction rate and product purity, the CO2 can be circularly used, and its isoforaxidin content in the extract of acanthopanax root is high, can be used for preparing medicine.

Description

The extracting method of Isofraxidin
Affiliated technical field
The present invention relates to a kind of extracting method of Isofraxidin, particularly a kind of method of extracting Isofraxidin with the CO 2 supercritical technology.
Background technology
The Araliaceae Radix Et Caulis Acanthopanacis Senticosi, it is the typical medicinal plant in China the Northeast, its activeconstituents is a lot, Radix Et Caulis Acanthopanacis Senticosi effective constituent Isofraxidin is researcher concern extremely both at home and abroad in recent years, report for work and contain this composition in recently a lot of cardiovascular agentes and Yang invigorating medicine the inside, domesticly look into new result and show, do not find to extract the research of Radix Et Caulis Acanthopanacis Senticosi Isofraxidin aspect with supercritical carbon dioxide extraction method.The research of extracts active ingredients aspect all is to adopt traditional solvent-extraction process in the relevant Radix Et Caulis Acanthopanacis Senticosi, because Isofraxidin content in Radix Et Caulis Acanthopanacis Senticosi is not high, extract, purify with ordinary method, workload is quite big, and solvent consumption is big, and foreign matter content height in the products therefrom, cost are also quite high, environmental pollution is big, is unsuitable for suitability for industrialized production.The world is looked into new result and is shown, from the Oleaceae plant, extract the existing bibliographical information of research of Isofraxidin with supercritical liquid extraction technique, this report mainly is the effect of extracting of the supercritical extraction of the different coumarin substances of comparative structure, belongs to the chemical analysis category.But the research of extracting Isofraxidin with this technology from Radix Et Caulis Acanthopanacis Senticosi does not see that the pertinent literature report is arranged.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, provide a kind of flow process simple, easy to operate, realize to separate simultaneously in extraction process, non-environmental-pollution is suitable for the Isofraxidin production technique of suitability for industrialized production.
The technical solution used in the present invention is: Radix Et Caulis Acanthopanacis Senticosi rhizome pulverizing → oven dry → supercritical carbon dioxide extraction → flash trapping stage → secondary separation → concentrated extract → vacuum-drying obtains the operational path of Isofraxidin.Advantage of the present invention is
1. the present invention adopts Isofraxidin in the supercritical carbon dioxide extraction method extraction Radix Et Caulis Acanthopanacis Senticosi, and it is fast to have an extraction rate, efficiency of pcr product height, the characteristics that carbonic acid gas can recycle.Be better than traditional solvent and extract Isofraxidin.
2. the present invention is raw material with the Radix Et Caulis Acanthopanacis Senticosi, adopts super critical CO 2 technology, and the relative content that makes Isofraxidin in the product is up to 64.34%, and yield can reach 0.5381 ‰ (Gu produce thing weight/raw material dry weights).In the whole process of production, solvent-oil ratio is little, non-environmental-pollution.
3. the present invention's no solvent residue does not aborning have " three wastes " discharging substantially, and environmentally safe is little to producers' toxicity, production safety coefficient height.
4. the present invention finished one and takes turns extraction and sepn process, production efficiency height in 3-5 hour.
Embodiment
Below embodiments of the invention are described in further detail:
Production process route of the present invention: Radix Et Caulis Acanthopanacis Senticosi rhizome pulverizing → oven dry → supercritical carbon dioxide extraction → flash trapping stage → secondary separation → concentrated extract → vacuum-drying obtains Isofraxidin.
The extracting method of described Isofraxidin is characterized in that: bake out temperature is 60 ℃, and drying time is 4-6 hour, and grinding particle size is the 60-80 order.
The extracting method of described Isofraxidin is characterized in that: adopt super critical CO 2 technology, the ethanol of 50%-80% is as entrainment agent, and extractor pressure is 25-30MPa, and temperature is 35-40 ℃.The flash trapping stage pressure tank is 5-10MPa, and temperature is 40-50 ℃, and secondary separating tank pressure is 5MPa, and temperature is 40-45 ℃, and extraction time is 3-5 hour.
The extracting method of described Isofraxidin is characterized in that: 45-55 ℃ of vacuum-drying temperature, and vacuum tightness-0.06~-0.08MPa.
Embodiment 1
It is about 60 orders that the Radix Et Caulis Acanthopanacis Senticosi rhizome is crushed to granularity, takes by weighing 180 grams, and bake out temperature is 60 ℃, and drying time is 6 hours.Drop in the extraction kettle oven dry back, and extraction conditions is: extracting pressure is 25MPa, and temperature is 35 ℃; Separation condition is: flash trapping stage still pressure is 6MPa, and temperature is 40 ℃, and secondary separating still pressure is 5MPa, and temperature is 45 ℃; 75% ethanol is done entrainment agent.Behind the dynamic operation 4 hours.In flash trapping stage still and secondary separating still, obtain Isofraxidin extracting solution 654ml, dense
Embodiment 2
It is about 70 orders that the Radix Et Caulis Acanthopanacis Senticosi rhizome is crushed to granularity, takes by weighing 180 grams, and bake out temperature is 60 ℃, and drying time is 5 hours.Drop in the extraction kettle oven dry back, and extraction conditions is: extracting pressure is 27MPa, and temperature is 40 ℃; Separation condition is: flash trapping stage still pressure is 6MPa, and temperature is 50 ℃, and secondary separating still pressure is 5MPa, and temperature is 45 ℃.65% ethanol is done entrainment agent.Behind the dynamic operation 4 hours.In flash trapping stage still and secondary separating still, obtain Isofraxidin extracting solution 735ml, concentrated extracting solution, 50 ℃ of temperature, vacuum-drying under vacuum tightness-0.07MPa, Isofraxidin pure substance yield is in the product: 0.5381 ‰.
Embodiment 3
It is about 80 orders that the Radix Et Caulis Acanthopanacis Senticosi rhizome is crushed to granularity, takes by weighing 180 grams, and bake out temperature is 60 ℃, and drying time is 4.5 hours.Drop in the extraction kettle oven dry back, and extraction conditions is: extracting pressure is 30MPa, and temperature is 50 ℃; Separation condition is: flash trapping stage still pressure is 6MPa, and temperature is 50 ℃, and secondary separating still pressure is 5MPa, and temperature is 45 ℃.55% ethanol is done entrainment agent.Behind the dynamic operation 5 hours.In flash trapping stage still and secondary separating still, obtain Isofraxidin extracting solution 668ml, concentrated extracting solution, 55 ℃ of temperature, vacuum-drying under vacuum tightness-0.06MPa, Isofraxidin pure substance yield is in the product: 0.5324 ‰.

Claims (4)

1, a kind of extracting method of Isofraxidin is characterized in that: Radix Et Caulis Acanthopanacis Senticosi rhizome pulverizing → oven dry → supercritical carbon dioxide extraction → flash trapping stage → secondary separation → concentrated extract → vacuum-drying obtains the operational path of Isofraxidin.
2, the extracting method of the described Isofraxidin of claim 1 is characterized in that: bake out temperature is 60 ℃, and drying time is 4-6 hour, and grinding particle size is the 60-80 order.
3, the extracting method of the described Isofraxidin of claim 1 is characterized in that: adopt super critical CO 2 technology, the ethanol of 50%-80% is as entrainment agent, and extractor pressure is 25-30MPa, and temperature is 35-40 ℃.The flash trapping stage pressure tank is 5-10MPa, and temperature is 40-50 ℃, and secondary separating tank pressure is 5MPa, and temperature is 40-45 ℃, and extraction time is 3-5 hour.
4, the extracting method of the described Isofraxidin of claim 1 is characterized in that: 45-55 ℃ of vacuum-drying temperature, and vacuum tightness-0.06~-0.08MPa.
CN02109476A 2002-04-10 2002-04-10 Process for extracting Isofraxidin Pending CN1450061A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN02109476A CN1450061A (en) 2002-04-10 2002-04-10 Process for extracting Isofraxidin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN02109476A CN1450061A (en) 2002-04-10 2002-04-10 Process for extracting Isofraxidin

Publications (1)

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CN1450061A true CN1450061A (en) 2003-10-22

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101851219A (en) * 2010-05-27 2010-10-06 东北林业大学 Method for preparing isofraxidin from acanthopanax senticosus rhizomes
CN108392506A (en) * 2018-05-23 2018-08-14 广东工业大学 The extracting method and pharmaceutical composition of a kind of wilsonii activity extract and its application
CN108484557A (en) * 2018-06-15 2018-09-04 东北林业大学 A method of extracting isofraxidin from wilsonii

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101851219A (en) * 2010-05-27 2010-10-06 东北林业大学 Method for preparing isofraxidin from acanthopanax senticosus rhizomes
CN108392506A (en) * 2018-05-23 2018-08-14 广东工业大学 The extracting method and pharmaceutical composition of a kind of wilsonii activity extract and its application
CN108484557A (en) * 2018-06-15 2018-09-04 东北林业大学 A method of extracting isofraxidin from wilsonii

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