CN104523784A - Method for extracting Chinese angelica extract - Google Patents
Method for extracting Chinese angelica extract Download PDFInfo
- Publication number
- CN104523784A CN104523784A CN201410824164.6A CN201410824164A CN104523784A CN 104523784 A CN104523784 A CN 104523784A CN 201410824164 A CN201410824164 A CN 201410824164A CN 104523784 A CN104523784 A CN 104523784A
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- CN
- China
- Prior art keywords
- radix angelicae
- angelicae sinensis
- chinese angelica
- extract
- sinensis extract
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- 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.)
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Classifications
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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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- 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
-
- 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
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention provides a method for extracting a Chinese angelica extract and belongs to an extraction method of traditional Chinese medicine active ingredients. The method for extracting the Chinese angelica extract comprises the following steps: cleaning and drying the Chinese angelica until the surface moisture content of the Chinese angelica is less than or equal to 0.5%, next, grinding the Chinese angelica into powder having the particle size of 50-100 microns, feeding the powder into an ethanol solution and performing microwave assisted extraction and ethanol extraction for 1-3 times, filtering while hot, recovering a yellowish-brown oily matter from the filtrate under reduced pressure, placing at a room temperature for 5-12 hours, taking the upper-layer oily matter, performing adsorption and desorption by use of macroporous resin to obtain high-purity Chinese angelica extract, and finally, drying to obtain light yellow powdery Chinese angelica extract. The content of active ingredient ligustilide in the Chinese angelica extract is greater than or equal to 7%. The method for extracting the Chinese angelica extract has the advantage that the extract finally obtained by virtue of ethanol extraction, microwave assisted extraction and adsorption and desorption by use of the macroporous resin is high in purity and short in extraction time, and the extraction process is safe and non-toxic.
Description
Technical field
The present invention relates to a kind of method extracting Radix Angelicae Sinensis extract, belong to Organic substance method of purification.
Background technology
When being classified as the dry root of Radix Angelicae Sinensis Angelica Sinensis (Oliv.) Diels, perennial herb, Herb has special fragrance.Main root tubbiness, loose meat, is divided into majority slightly to draw money on credit root below.Stem is upright, band purple.Perennial herb is high 0.4 ~ 1 meter.Stem is upright, and band purple, has obvious longitudinal grin straight trough, Glabrous.Dry root total length about 10 ~ 25 centimetres, height 3 ~ 10 centimetres, appearance taupe brown or sepia, all tools indulge wrinkle, return body slightly cylindrical, body and uneven, and it is lower the Radix Angelicae Sinensis of 3 ~ 5 or more.Radix Angelicae Sinensis is upper coarse and lower fine, many distortions, table and have the fibrous root vestige of goose pimples shape.Gas delicate fragrance is dense, and sweet and slightly bitter taste is pungent.General must cultivation just can be gathered for 3 years, and autumn end takes root.
Present custom adopts higher-quality supercritical fluid extraction, and a kind of supercritical fluid that utilizes carrys out the technology of separate substance for mobile phase.CO
2it is solvent the most frequently used in supercritical fluid technology.Supercritical CO
2fluid has the biphase dual characteristics of gas, liquid concurrently, has both had the high diffusivity coefficient suitable with gas and low viscosity, has again the density close with liquid and to material.The principle of supercritical carbon dioxide extraction separation process utilizes supercritical carbon dioxide to have special dissolution to some special natural product, utilize the solvability of supercritical carbon dioxide and the relation of its density, namely utilize pressure and temperature to carry out the impact of supercritical carbon dioxide solvability.In the supercritical state, supercritical carbon dioxide is contacted with material to be separated, make it selectively the composition of polarity size, boiling point height and molecular size range be extracted successively.Certainly, the extract that corresponding each pressure limit obtains can not be single, but controlled condition can obtain the blending constituent of optimal proportion, then the method by decompression, intensification makes supercritical fluid become common gases, be extracted material then to separate out completely or substantially, thus reach the object of separating-purifying, so supercritical fluid carbon dioxide extraction process is combined by extraction and fractionation.
The chemical composition of Radix Angelicae Sinensis mainly comprises ligustilide class and isomeric compound, Coumarins, polysaccharide, flavonoid and organic acid etc.Radix Angelicae Sinensis, containing volatile oil composition and organic acid, is mainly the compositions such as succinic acid, Yan acid, uracil, adenine, ligustilide, vitamin B12, vitamin E, sitoesterol, folinic acid, butylidenephthalide, ferulic acid/choline, 5-hy droxy furan aldehyde, trace element (as zinc, copper, ferrum, manganese, potassium, sodium, calcium etc.), phospholipid and vitamin A.The active component of Radix Angelicae Sinensis for having calmness, antiinflammatory, vitamin antagonist E deficiency disease act on.The chemical composition of Radix Angelicae Sinensis extract mainly comprises ligustilide class and isomeric compound, Coumarins, polysaccharide, flavonoid and organic acid etc.The active component of Radix Angelicae Sinensis has calmness, antiinflammatory, vitamin antagonist E deficiency disease act on.The effective ingredient of Radix Angelicae Sinensis extract is ligustilide and normal-butyl.
Summary of the invention
The shortcomings such as extraction cost is high in order to solve, the purity of extraction of substance is low.The present invention takes microwave radiation exaraction and macroporous resin adsorption and parsing to obtain the high Radix Angelicae Sinensis extract of purity to Radix Angelicae Sinensis.
Technical scheme of the present invention is: provide a kind of extracting method, ligustilide >=7% in this Radix Angelicae Sinensis extract, preferred ligustilide >=9%.
Radix Angelicae Sinensis extract method step of the present invention is: the Radix Angelicae Sinensis adopting more than 3 years summers of plantation, late autumn or early winter, removing fibrous root and silt, adopts to dry in the shade, to dry or the mode such as cold drying makes Radix Angelicae Sinensis surface moisture≤0.5%; Adopt machinery or manual physical method to be ground into the powder that particle diameter is 50 ~ 100um, be then stirred well in alcoholic solution by powder, at 50 ~ 150 DEG C, adopt microwave radiation exaraction, microwave power is 250 ~ 400w, and the microwave extraction time is 20 ~ 60min; Getting filtrate uses 20% ~ 50% (v/v) ethanol to extract 1 ~ 3 time at 50 ~ 70 DEG C again, and each extraction time is 20min ~ 50min; Filtered while hot, filtrate by reclaim under reduced pressure to without alcohol taste (temperature is 20 ~ 30 DEG C), obtain yellowish-brown grease, at room temperature place 5 ~ 12h, faint yellow solid content is separated out in bottom, get upper strata grease, obtain the high Radix Angelicae Sinensis extract of purity through macroporous resin adsorption and parsing, final drying obtains light yellow powder Radix Angelicae Sinensis extract.Effective ingredient ligustilide >=7% in Radix Angelicae Sinensis extract.
Concrete, the type of above-mentioned macroporous resin is D101, AB-8, A20, HPD-400, HPD-400A or HPD-450.Preferably, the type of macroporous resin is D101, HPD-400A or HPD-450.
Particularly, when above-mentioned employing macroporous resin adsorption and parsing, eluent is the ethanol of 20 ~ 40% (v/v).
Alcohol steep methods combining microwave radiation exaraction of the present invention, makes Organic substance in Chinese Angelica Root to be extracted further.Macroporous resin is finally adopted to carry out adsorbing or resolving the purity of Radix Angelicae Sinensis extract is improved.The present invention adopts the form of above-mentioned combined extracting, and the material purity that extraction obtains is high, extraction time is short, and in whole leaching process, the ethanol of low-purity is as solvent, extractant or eluant simultaneously, nontoxic, pollution-free; There is obvious economic benefit and environmental benefit.
Detailed description of the invention
Adopt plantation after 3 years summer, Qiu Mo or early winter excavate Radix Angelicae Sinensis, removing fibrous root and silt, mode makes Radix Angelicae Sinensis root moisture≤1% then to clean up rear employings oven dry, cold drying or dry in the shade etc.
By above-mentioned Radix Angelicae Sinensis root more further drying make its moisture≤0.5%, adopt machinery or manual physical method to be ground into the powder that particle diameter is 50 ~ 100um; Then be stirred well in alcoholic solution by powder, at 50 ~ 150 DEG C, adopt microwave radiation exaraction, microwave power is 250 ~ 400w, and the microwave extraction time is 20 ~ 60min; Getting filtrate uses 20% ~ 50% (v/v) ethanol to extract 1 ~ 3 time at 50 ~ 70 DEG C again, and each extraction time is 20min ~ 50min; Filtered while hot, filtrate by reclaim under reduced pressure to without alcohol taste (temperature is 20 ~ 30 DEG C), obtain yellowish-brown grease, at room temperature place 5 ~ 12h, faint yellow solid content is separated out in bottom, get upper strata grease, obtain the high Radix Angelicae Sinensis extract of purity through macroporous resin adsorption and parsing, final drying obtains light yellow powder Radix Angelicae Sinensis extract.Effective ingredient ligustilide >=7% in Radix Angelicae Sinensis extract.
embodiment 1
Adopt the Radix Angelicae Sinensis in plantation summer after 3 years, removing fibrous root and silt, then cleaning up rear employing temperature is that 30 ~ 50 DEG C of oven drying at low temperatures make Radix Angelicae Sinensis root moisture 0.2%.Then above-mentioned Radix Angelicae Sinensis root is ground into the powder that particle diameter is 50 ~ 100um in pulverizer, powder weight is 240g.Above-mentioned powder is stirred well to 1700ml, concentration is in 40% (v/v) alcoholic solution, at 70 DEG C, adopt microwave radiation exaraction, microwave power is 250w, and the microwave extraction time is 45min; Then after the filtrate of gained extracts 40min with 20% (v/v) ethanol at 70 DEG C, filtered while hot, filtrate by reclaim under reduced pressure to without alcohol taste, obtain yellowish-brown grease, at room temperature place 7h, faint yellow solid content is separated out in bottom, gets upper strata grease, obtains the high Radix Angelicae Sinensis extract of purity through D101 macroporous resin adsorption and parsing, eluting and drying.In Radix Angelicae Sinensis extract, effective ingredient ligustilide is 8.9%.
embodiment 2
Adopt the Radix Angelicae Sinensis of plantation early winter after 3 years, removing fibrous root and silt, then clean up the rear mode of drying in the shade of ventilating that adopts and make Radix Angelicae Sinensis root moisture 0.9%.Then above-mentioned Radix Angelicae Sinensis root is ground into the powder that particle diameter is 50 ~ 100um in pulverizer, powder weight is 270g.Above-mentioned powder is stirred well to 1900ml, concentration is in 50% (v/v) alcoholic solution, at 110 DEG C, adopt microwave radiation exaraction, microwave power is 300w, and the microwave extraction time is 25min; Then gained filtrate with 50% (v/v) ethanol 60 DEG C extract 20min and then with 40% (v/v) ethanol 70 DEG C extraction 30min after, filtered while hot, filtrate by reclaim under reduced pressure to without alcohol taste, obtain yellowish-brown grease, at room temperature place 12h, faint yellow solid content is separated out in bottom, gets upper strata grease, obtains the high Radix Angelicae Sinensis extract of purity through AB-8 macroporous resin adsorption and parsing, eluting and drying.In Radix Angelicae Sinensis extract, effective ingredient ligustilide is 9.7%.
embodiment 3
Adopt the Radix Angelicae Sinensis in plantation late autumn after 3 years, removing fibrous root and silt, the mode then cleaning up rear employing oven drying at low temperature makes Radix Angelicae Sinensis root moisture 0.4%.Then above-mentioned Radix Angelicae Sinensis root is ground into the powder that particle diameter is 50 ~ 100um in pulverizer, powder weight is 300g.Above-mentioned powder is stirred well to 2000ml, concentration is in 40% (v/v) alcoholic solution, at 130 DEG C, adopt microwave radiation exaraction, microwave power is 400w, and the microwave extraction time is 15min; Then gained filtrate with 50% (v/v) ethanol 50 DEG C extract 30min and then with 20% (v/v) ethanol 50 DEG C extraction 50min after, filtered while hot, filtrate by reclaim under reduced pressure to without alcohol taste, obtain yellowish-brown grease, at room temperature place 10h, faint yellow solid content is separated out in bottom, gets upper strata grease, obtains the high Radix Angelicae Sinensis extract of purity through A20 macroporous resin adsorption and parsing, eluting and drying.In Radix Angelicae Sinensis extract, effective ingredient ligustilide is 10.4%.
Above-described embodiment is only in order to illustrate technical scheme of the present invention; but not design of the present invention and protection domain are limited; those of ordinary skill in the art modifies to technical scheme of the present invention or equivalent replacement; and not departing from aim and the scope of technical scheme, it all should be encompassed in right of the present invention.
Claims (7)
1. extract a method for Radix Angelicae Sinensis extract, it specifically comprises the following steps: after Radix Angelicae Sinensis cleans up, and adopts to dry in the shade, to dry or the mode such as cold drying makes Radix Angelicae Sinensis surface moisture≤0.5%; Adopt machinery or manual physical method to be ground into the powder that particle diameter is 50 ~ 100um, be then stirred well in alcoholic solution by powder, at 50 ~ 150 DEG C, adopt microwave radiation exaraction, microwave power is 250 ~ 400w, and the microwave extraction time is 20 ~ 60min; Getting filtrate uses 20% ~ 50% (v/v) ethanol to extract 1 ~ 3 time at 50 ~ 70 DEG C again, and each extraction time is 20min ~ 50min; Filtered while hot, filtrate by reclaim under reduced pressure to without alcohol taste, obtain yellowish-brown grease, at room temperature place 5 ~ 12h, faint yellow solid content is separated out in bottom, get upper strata grease, obtain the high Radix Angelicae Sinensis extract of purity through macroporous resin adsorption and parsing, final drying obtains light yellow powder Radix Angelicae Sinensis extract.
2. a kind of method extracting Radix Angelicae Sinensis extract according to claim 1, is characterized in that: described when be classified as the Radix Angelicae Sinensis root of planting more than 3 years summers, late autumn or early winter.
3. a kind of method extracting Radix Angelicae Sinensis extract according to claim 1, is characterized in that: the type of described macroporous resin is D101, AB-8, A20, HPD-400, HPD-400A or HPD-450.
4. a kind of method extracting Radix Angelicae Sinensis extract according to claim 1, is characterized in that: the type of described macroporous resin is D101, HPD-400A or HPD-450.
5. a kind of method extracting Radix Angelicae Sinensis extract according to claim 1, is characterized in that: when described macroporous resin adsorption and parsing, eluent is the ethanol of 20 ~ 40% (v/v).
6. a kind of method extracting Radix Angelicae Sinensis extract according to claim 1, is characterized in that: ligustilide >=7% in described Radix Angelicae Sinensis extract.
7. a kind of method extracting Radix Angelicae Sinensis extract according to claim 1, is characterized in that: ligustilide >=9% in described Radix Angelicae Sinensis extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410824164.6A CN104523784A (en) | 2014-12-26 | 2014-12-26 | Method for extracting Chinese angelica extract |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410824164.6A CN104523784A (en) | 2014-12-26 | 2014-12-26 | Method for extracting Chinese angelica extract |
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| CN104523784A true CN104523784A (en) | 2015-04-22 |
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| CN201410824164.6A Pending CN104523784A (en) | 2014-12-26 | 2014-12-26 | Method for extracting Chinese angelica extract |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546963A (en) * | 2014-12-26 | 2015-04-29 | 高俊丽 | Method for extracting extract from angelica sinensis |
| CN108991414A (en) * | 2018-06-26 | 2018-12-14 | 襄阳三珍生态农业有限公司 | A kind of production technology of Radix Angelicae Sinensis acorn nut vermicelli |
| CN109867598A (en) * | 2017-12-01 | 2019-06-11 | 北京国康本草物种生物科学技术研究院有限公司 | Radix Angelicae Sinensis extraction process of effective component and its extract |
| CN113004975A (en) * | 2021-03-19 | 2021-06-22 | 湖南安邦制药股份有限公司 | Method for extracting mixed volatile oil of angelica and fingered citron |
-
2014
- 2014-12-26 CN CN201410824164.6A patent/CN104523784A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546963A (en) * | 2014-12-26 | 2015-04-29 | 高俊丽 | Method for extracting extract from angelica sinensis |
| CN109867598A (en) * | 2017-12-01 | 2019-06-11 | 北京国康本草物种生物科学技术研究院有限公司 | Radix Angelicae Sinensis extraction process of effective component and its extract |
| CN108991414A (en) * | 2018-06-26 | 2018-12-14 | 襄阳三珍生态农业有限公司 | A kind of production technology of Radix Angelicae Sinensis acorn nut vermicelli |
| CN113004975A (en) * | 2021-03-19 | 2021-06-22 | 湖南安邦制药股份有限公司 | Method for extracting mixed volatile oil of angelica and fingered citron |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150422 |
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| WD01 | Invention patent application deemed withdrawn after publication |