CN106176849A - A kind of subcritical fluid techniques extracts the method for Yu's Essential Oil of Radix Angelicae Dahuricae - Google Patents
A kind of subcritical fluid techniques extracts the method for Yu's Essential Oil of Radix Angelicae Dahuricae Download PDFInfo
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- CN106176849A CN106176849A CN201610534848.1A CN201610534848A CN106176849A CN 106176849 A CN106176849 A CN 106176849A CN 201610534848 A CN201610534848 A CN 201610534848A CN 106176849 A CN106176849 A CN 106176849A
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- organic solvent
- radix angelicae
- angelicae dahuricae
- essential oil
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
- A61K36/232—Angelica
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- General Health & Medical Sciences (AREA)
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of method using subcritical fluid techniques to extract Yu's Essential Oil of Radix Angelicae Dahuricae, the method that the present invention uses subcritical fluids to prepare Yu's Essential Oil of Radix Angelicae Dahuricae is carried out under mesophilic condition, do not destroy the active substance of medical material, solve because high temperature causes volatile oil inactivation and rotten problem, recycling of solvent can be realized simultaneously, improve raw-material utilization rate, reduce energy consumption, shorten the production cycle, be suitable for industrialized production.
Description
Technical field
The invention belongs to extracting technique of Chinese medicine technical field, be specifically related to a kind of subcritical fluid techniques extraction Yu Baizhi and wave
The method of hair oil.
Background technology
The Radix Angelicae Dahuricae is the dry root of the samphire Radix Angelicae Dahuricae or Radix angelicae dahuricae, is one of tcm clinical practice common medicine, and it begins to be recorded in,
Shennong's Herbal, warm in nature, acrid in the mouth, have dispel the wind, dehumidify, circulation of qi promoting, pain relieving, the skin ulcer that disappears, the effect stopped blooding, improve looks, be used for treating
Headache due to common cold, supraorbital bone pain, nasal sinusitis, toothache, skin infection swells and ache, and research shows, the Radix Angelicae Dahuricae has antiinflammatory, antipyretic, analgesia, disease-resistant former
The effect of microorganism, can suppress psoriasis, treats vitiligo, has the parasympathetic effect of antagonism, have relieving spasm to stop pain effect
Deng, the commodity Radix Angelicae Dahuricae mainly has Qi Baizhi, Yu Baizhi, Radix angelicae dahuricae, angelica anomala, and in the Radix Angelicae Dahuricae, contained chemical composition is with volatile oil and tonkabean
Element class is main.Modern pharmacology research shows that the abundant volatile oil component contained by Yu Baizhi is that it plays the main of pharmacological action
One of material base, Yu's Essential Oil of Radix Angelicae Dahuricae complex chemical composition, its main component is alkanols and carbene compounds, such as 1-ten
Dialkanol, 1-tetradecanol, a-pinene etc., this two compounds accounts for the 62-78% of whole volatile oil, is secondly saturated hydrocarbons
And organic acid, in addition with a small amount of aldehyde, ketone, ester and benzene derivate etc..
Although narcotic analgesics analgesic effect is notable, but its serious toxic and side effects makes people hang back, and Chinese medicine is the most not
So, the diaphoretic medicine that the Radix Angelicae Dahuricae is commonly used as clinic, in treating various types of pain symptoms, effect is preferable, especially at treatment head
Portion's pain and skin infection swell and ache aspect, and the most indispensable good medicine simply, experiment results proved, Essential Oil of Radix Angelicae Dahuricae analgesic effect is true
Cut, and length of holding time, and there is obvious maincenter sedation.The toxicity of Essential Oil of Radix Angelicae Dahuricae is low, and safety range is wide, and research is sent out
Existing Essential Oil of Radix Angelicae Dahuricae analgesia, sedation effect is obvious, and without physical dependence effect, has broad application prospects.
Essential Oil of Radix Angelicae Dahuricae extracting method is the most single, and now great majority use two kinds of extracting method, steam distillation and
Supercritical carbon dioxide process, steam distillation application is more universal, and the volatile oil purity prepared in this way is higher, low boiling
The volatile component content of point is the highest, but in this way, angelica root easily gelatinizing, it is unfavorable for operation, and volatilizees
Oil and air and light Long contact time, meeting gradually oxidation deterioration, form resinoid, yield is relatively low, supercritical carbon dioxide
Abstraction technique has the good period, and efficiency is high, and operation temperature is low, the advantage that can preserve the effective ingredient of medical material in a large number, but to having
The volatile ingredient that a little polarity are big or volatile oil and lower boiling volatile oil with bonding state existence can not be extracted efficiently, and
And this technology is higher to equipment requirements, it is also difficult at present popularize, in view of this, it is an object of the invention to be for existing skill
The deficiency of art, it is provided that a kind of method utilizing subcritical fluid techniques to prepare Essential Oil of Radix Angelicae Dahuricae, subcritical fluid techniques is as elder generation
The extractive technique entered, causes power consumption little, destroys less to volatile oil, and organic solvent recycles etc. a little, at volatile oil is drawn
Upper having increasingly is widely applied.
The present invention, with Yuzhou genuine traditional Chinese medicine material Yu's Radix Angelicae Dahuricae as object of study, uses subcritical fluids to prepare Yu's Essential Oil of Radix Angelicae Dahuricae
Method carry out under mesophilic condition, do not destroy the active substance of medical material, solve because high temperature causes volatile oil inactivation with rotten
Problem, simultaneously can realize recycling of solvent, improve raw-material utilization rate, reduce energy consumption, shorten the production cycle, suitable
Close industrialized production.
Summary of the invention
It is an object of the invention to overcome the determination that Essential Oil of Radix Angelicae Dahuricae extracting method is single, extraction ratio is low, it is provided that a kind of right
Volatile oil destroys less, and the subcritical fluid techniques that organic solvent recycles extracts the method for Yu's Essential Oil of Radix Angelicae Dahuricae, the present invention
Adopt the following technical scheme that
A kind of subcritical fluid techniques extracts the method for Yu's Essential Oil of Radix Angelicae Dahuricae, and it comprises the following steps:
A, pretreatment: Yu Baizhi pulverizes 60-120 mesh, obtains Yu's Dahurian Angelica Root, Yu's Dahurian Angelica Root is loaded thin,tough silk bag and puts into extractor
In, preheating experimental facilities, to 60-75 DEG C, starts vacuum pump and extractor and separation pressure inside the tank is evacuated to-0.10MPa；
B extracts: opens extractor solvent injection valve, 3-5cm above injection organic solvent to solvent submergence all thin,tough silk bag, opens heat
Water circulation system pump, maintains extraction temperature 60-75 DEG C, and extracting pressure 0.2-0.8MPa extracts, and obtains oil soluble mixture；
C, precipitation separate: open extractor sample output valve, knockout drum injection valve, and described oil soluble mixture is separated by extractor press-in
After tank, starting compressor, condenser system, oil soluble mixture carries out heat up pressurization and carrying out precipitation treatment, pressure tank to be separated is down to
0.1MPa-0.20MPa, starts vacuum pump, accelerates precipitation with compressor linkage and separates, and obtains the organic solvent of liquid and liquid
Yu's Essential Oil of Radix Angelicae Dahuricae；
D, collection product, described liquid organic solvent enters holding vessel and recycles, and opens knockout drum outlet valve, collects described
Yu's Essential Oil of Radix Angelicae Dahuricae, repeat above-mentioned extraction 3-4 time, reclaim organic solvent and recycle；
E, process residue, collect residue carry out coumarin substances extraction；
Described thin,tough silk bag mesh number is 200-300 mesh.
Described extraction time is 30-90 minute.
Described organic solvent is one or more in propane, butane, ether, acetone.
The recovery method of described liquid organic solvent is as follows: open compressor in precipitation separation process and recirculated water is carried out
Compression and condensation, collect organic solvent gas and be compressed and condense, obtain liquid organic solvent and recycle.
Beneficial effects of the present invention: use subcritical fluid extraction, compared with vapor extraction, have with short production cycle,
Efficiency is high, and yield and quality is high a little, compared with supercritical carbon dioxide extraction, has industrialization degree high, and production cost is low
Advantage product of the present invention, production technology is simple, and constant product quality, low temperature to extract activity destroy little, energy consumption
Less, yield high, be suitable for large-scale production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
A kind of subcritical fluid techniques extracts the method for Yu's Essential Oil of Radix Angelicae Dahuricae, and it comprises the steps:
A, pretreatment: Yu Baizhi pulverizes 80 mesh, obtains Yu's Dahurian Angelica Root, Yu Dahurian Angelica Root 5kg is loaded 5 240 mesh thin,tough silk bags and throws
Entering in extractor, preheating experimental facilities, to 65 DEG C, starts vacuum pump and extractor and separation pressure inside the tank is evacuated to-0.10MPa；
B extracts: opens extractor solvent injection valve, 5cm above injection butane to solvent submergence all thin,tough silk bag, opens hot water circuit
Systems pumps, maintains extraction temperature 65 DEG C, and extracting pressure 0.4MPa extracts, and extraction time is 60 minutes, obtains oil soluble mixing
Thing；
C, precipitation separate: open extractor sample output valve, knockout drum injection valve, and described oil soluble mixture is separated by extractor press-in
After tank, starting compressor, condenser system, oil soluble mixture carries out heat up pressurization and carrying out precipitation treatment, pressure tank to be separated is down to
0.1MPa, starts vacuum pump, accelerates precipitation with compressor linkage and separates, and obtains the butane of liquid and the Yu Baizhi volatilization of liquid
Oil；
D, collection product: described liquefied butane enters holding vessel and recycles, and opens knockout drum outlet valve, Yu described in collection
Essential Oil of Radix Angelicae Dahuricae, repeats above-mentioned extraction 3 times, collects Yu Essential Oil of Radix Angelicae Dahuricae 278ml, and extraction yield is 5.56%；
E, process residue: collect residue 4.5kg carry out coumarin substances extraction；
Embodiment 2
A, pretreatment: Yu Baizhi pulverizes 100 mesh, obtains Yu's Dahurian Angelica Root, Yu Dahurian Angelica Root 5kg is loaded 5 240 mesh thin,tough silk bags and throws
Entering in extractor, preheating experimental facilities, to 60 DEG C, starts vacuum pump and extractor and separation pressure inside the tank is evacuated to-0.10MPa；
B extracts: opens extractor solvent injection valve, 5cm above injection butane to solvent submergence all thin,tough silk bag, opens hot water circuit
Systems pumps, maintains extraction temperature 70 DEG C, and extracting pressure 0.4MPa extracts, and extraction time is 60 minutes, obtains oil soluble mixing
Thing；
C, precipitation separate: open extractor sample output valve, knockout drum injection valve, and described oil soluble mixture is separated by extractor press-in
After tank, starting compressor, condenser system, oil soluble mixture carries out heat up pressurization and carrying out precipitation treatment, pressure tank to be separated is down to
0.1MPa, starts vacuum pump, accelerates precipitation with compressor linkage and separates, and obtains the butane of liquid and the Yu Baizhi volatilization of liquid
Oil；
D, collection product: described liquefied butane enters holding vessel and recycles, and opens knockout drum outlet valve, Yu described in collection
Essential Oil of Radix Angelicae Dahuricae, repeats above-mentioned extraction 4 times, merges and collects Yu Essential Oil of Radix Angelicae Dahuricae 317ml, and extraction yield is 6.34%；
E, process residue, collect residue 4.5kg carry out coumarin substances extraction；
Embodiment 3
A kind of subcritical fluid techniques extracts the granting of Yu's Essential Oil of Radix Angelicae Dahuricae, and it comprises the following steps:
A, pretreatment: take Yu Baizhi and pulverize 120 mesh, obtain Yu's Dahurian Angelica Root, be respectively charged into 5 240 mesh thin,tough silk by Yu Dahurian Angelica Root 5kg
Bag also puts in extractor, preheating experimental facilities to 60 DEG C, start vacuum pump by extractor and separate pressure inside the tank be evacuated to-
0.10MPa；
B extracts, and opens extractor solvent injection valve, 5cm above injection organic solvent to solvent submergence all thin,tough silk bag, opens hot water
Blood circulation pump, maintains extraction temperature 65 DEG C, and extracting pressure 0.6MPa extracts, and extraction time is 60 minutes, obtains oil soluble
Mixture；
C, precipitation separate: open extractor sample output valve, knockout drum injection valve, and described oil soluble mixture is separated by extractor press-in
After tank, starting compressor, condenser system, oil soluble mixture carries out heat up pressurization and carrying out precipitation treatment, pressure tank to be separated is down to
0.1MPa, starts vacuum pump, accelerates precipitation with compressor linkage and separates, and the Yu Baizhi of the organic solvent and liquid that obtain liquid waves
Hair oil；
D, collection product, described liquid organic solvent enters holding vessel and recycles, and opens knockout drum outlet valve, collects described
Yu's Essential Oil of Radix Angelicae Dahuricae, repeat the above steps extract 3 times, merge collect Yu Essential Oil of Radix Angelicae Dahuricae 292ml, extraction yield is 5.84%；
E, process residue, collect residue 4.5kg carry out coumarin substances extraction.
Claims (5)
1. the method that a subcritical fluid techniques extracts Yu's Essential Oil of Radix Angelicae Dahuricae, it is characterised in that it comprises the following steps:
A, pretreatment: Yu Baizhi pulverizes 60-120 mesh, obtains Yu's Dahurian Angelica Root, Yu's Dahurian Angelica Root is loaded thin,tough silk bag and puts into extractor
In, preheating experimental facilities, to 60-75 DEG C, starts vacuum pump and extractor and separation pressure inside the tank is evacuated to-0.10MPa；
B extracts: opens extractor solvent injection valve, 3-5cm above injection organic solvent to solvent submergence all thin,tough silk bag, opens heat
Water circulation system pump, maintains extraction temperature 60-75 DEG C, and extracting pressure 0.2-0.8MPa extracts, and obtains oil soluble mixture；
C, precipitation separate: open extractor sample output valve, knockout drum injection valve, and described oil soluble mixture is separated by extractor press-in
After tank, starting compressor, condenser system, oil soluble mixture carries out heat up pressurization and carrying out precipitation treatment, pressure tank to be separated is down to
0.1MPa-0.20MPa, starts vacuum pump, accelerates precipitation with compressor linkage and separates, and obtains the organic solvent of liquid and liquid
Yu's Essential Oil of Radix Angelicae Dahuricae；
D, collection product: described liquid organic solvent reclaims and enters holding vessel recycling, opens knockout drum outlet valve, collects
Described Yu's Essential Oil of Radix Angelicae Dahuricae, repeats above-mentioned extraction 3-4 time；
E, process residue: collect residue carry out coumarin substances extraction.
2. thin,tough silk bag as claimed in claim 1, it is characterised in that described thin,tough silk bag mesh number is 200-300 mesh.
Extract the most as claimed in claim 1, it is characterised in that described extraction time is 30-90 minute.
4. organic solvent as claimed in claim 1, it is characterised in that described organic solvent be propane, butane, ether, third
One or more in ketone.
5. organic solvent as claimed in claim 1 reclaims, it is characterised in that the recovery method of described liquid organic solvent is such as
Under: precipitation separation process is opened compressor and recirculated water and is compressed and condenses, collect organic solvent gas be compressed and
Condensation, obtains liquid organic solvent and recycles.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108251218A (en) * | 2018-02-11 | 2018-07-06 | 安阳工学院 | A kind of method of highly selective extraction north Chinese mugwort essential oil |
| CN110305734A (en) * | 2019-07-03 | 2019-10-08 | 亳州职业技术学院 | A kind of extraction process of root of Dahurain angelica leaf volatile oil |
| CN115282192A (en) * | 2022-09-13 | 2022-11-04 | 四川大学华西医院 | Composition with anti-inflammatory and analgesic effects, experiment and preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105368573A (en) * | 2015-11-24 | 2016-03-02 | 郑州雪麦龙食品香料有限公司 | Method for preparing nutmeg oleoresin by using subcritical fluid |
| CN105505583A (en) * | 2015-11-24 | 2016-04-20 | 郑州雪麦龙食品香料有限公司 | A method of extracting bay leaf oil from bay leaves with subcritical n-butane fluid |
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2016
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105368573A (en) * | 2015-11-24 | 2016-03-02 | 郑州雪麦龙食品香料有限公司 | Method for preparing nutmeg oleoresin by using subcritical fluid |
| CN105505583A (en) * | 2015-11-24 | 2016-04-20 | 郑州雪麦龙食品香料有限公司 | A method of extracting bay leaf oil from bay leaves with subcritical n-butane fluid |
Non-Patent Citations (1)
| Title |
|---|
| 马逾英，等: "白芷挥发油的研究进展", 《中华中医药学会第九届中药鉴定学术会议论文集》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108251218A (en) * | 2018-02-11 | 2018-07-06 | 安阳工学院 | A kind of method of highly selective extraction north Chinese mugwort essential oil |
| CN108251218B (en) * | 2018-02-11 | 2021-06-15 | 安阳工学院 | Method for extracting artemisia vulgaris essential oil with high selectivity |
| CN110305734A (en) * | 2019-07-03 | 2019-10-08 | 亳州职业技术学院 | A kind of extraction process of root of Dahurain angelica leaf volatile oil |
| CN115282192A (en) * | 2022-09-13 | 2022-11-04 | 四川大学华西医院 | Composition with anti-inflammatory and analgesic effects, experiment and preparation method |
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Application publication date: 20161207 |