CN102503889A - Method for extracting asimilobine - Google Patents
Method for extracting asimilobine Download PDFInfo
- Publication number
- CN102503889A CN102503889A CN2011103037019A CN201110303701A CN102503889A CN 102503889 A CN102503889 A CN 102503889A CN 2011103037019 A CN2011103037019 A CN 2011103037019A CN 201110303701 A CN201110303701 A CN 201110303701A CN 102503889 A CN102503889 A CN 102503889A
- Authority
- CN
- China
- Prior art keywords
- extracting
- extraction
- crystallization
- lobine
- sago
- 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
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Seasonings (AREA)
Abstract
The invention relates to a method for extracting asimilobine, comprising the following steps: grinding raw materials into 20-40 meshes, ammoniating for 2-6 hours, adding into an extraction kettle, extracting by using supercritical CO2 for 2-4 hours by using methanol as the entrainer, analyzing to obtain extract, adding activated carbon to destain, filtering to obtain destaining solution, concentrating the destaining solution into extract, dissolving by using acid water, filtering, washing cation exchange resin in filtrate by using deionized water until the cation exchange resin is neutral, eluting by using alkaline alcohol solution, carrying out reduced pressure distillation to eluent, adjusting the pH value to 10-11, standing for crystallizing, filtering to remove crystal, recrystallizing by using acetone, and drying the crystal to obtain the product. The process for extracting the asimilobine is simple and easy to operate, causes less pollution and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of process for extracting of effective ingredients in plant, is a kind of process for extracting of Ah's sago lobine specifically.
Background technology
Ah's sago lobine belongs to the aporphine alkaloid compounds, white block crystallization, and mp.175～177 ℃ derive from annonaceae OX-heart sweetsop
Annona retieulataThe leaf of L.Ah's sago lobine is chloroquine sensitive strain D-6 (950) to the ED50 (ng/ml) of plasmodium falciparum, anti-chloroquine strain W-2 (470); To shrinking restraining effect is arranged, can be used as the 5-hydroxytryptamine receptor antagonist by serotonin inductive rabbit isolated aorta.
OX-heart sweetsop is Magnoliales (Magnoliales) annonaceae (Annonaceae) arbor, originates in the high altitude localities of tropical America free of frost, and extensively plant with the Shiqi fruit each department, continent.
At present, the domestic process for extracting related patent U.S. Patent No. report that does not still have Ah's sago lobine.
Summary of the invention
The technical problem that the present invention will solve provides a kind of process for extracting of Ah's sago lobine, and technological operation is simple, is easy to realize suitability for industrialized production.
In order to solve the problems of the technologies described above, the objective of the invention is to realize like this:
(1) getting OX-heart sweetsop dry leave is raw material, is crushed to the 20-40 order, ammonification 2-6 hour, add extraction kettle, and adopt supercritical CO
2Extraction is an entrainment agent with methyl alcohol, extracts 2-4 hour, resolves and obtains extraction liquid;
(2) above-mentioned extraction liquid adds the activated carbon decolorizing of the 0.8-1% of its volume, filters and obtains destainer, and destainer is concentrated into medicinal extract;
(3) above-mentioned medicinal extract dissolves with sour water, filters, and Zeo-karb on the filtrating is washed till neutrality with deionized water earlier, uses the alkaline alcohol solution wash-out again, and the elutriant concentrating under reduced pressure is transferred pH10-11, places crystallization, filters and obtains crystallization;
(4) above-mentioned crystallization refluxes with acetone and dissolves, and filtered while hot is put cold crystallization, leaches crystallizing and drying and promptly gets product.
Supercritical CO in the said step (1)
2Extraction temperature is 50-60 ℃, and extracting pressure is 30-38MPa, and the separating still temperature is 30-45 ℃, and pressure is 4-8MPa, CO
2Flow is 2-5ml/g raw material/min, and the volume percent that the entrainment agent consumption accounts for total extraction solvent is 3-6%.
Sour water is hydrochloric acid or the aqueous sulfuric acid of 3-5% in the said step (3).
A kind of in the said step (3) among the optional D151 of Zeo-karb, HZD-2 or the HD-8.
Said step (3) neutral and alkali alcoholic solution is the ethanolic soln of pH9-11, and concentration is 75-90%.
In sum, there is following advantage in the present invention: supercritical carbon dioxide extraction impurity is few, efficient is high; Adopted the exchange resin purifying, treatment capacity is big, and technology is simple to operation, and effect is better than extraction, has realized the industriallization purpose.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1:
Get OX-heart sweetsop dry leave raw material 1kg, be crushed to 20 orders, add 500ml ammoniacal liquor ammonification 4 hours, add extraction kettle, adopt supercritical CO
2Extraction is an entrainment agent with methyl alcohol, and the volume percent that the entrainment agent consumption accounts for total extraction solvent is 5%, and extraction temperature is 55 ℃, and extracting pressure is 38MPa, and the separating still temperature is 40 ℃, and pressure is 6MPa, CO
2Flow is 3ml/g raw material/min, extracts 3 hours, resolves and to obtain extraction liquid, adds 0.8% activated carbon decolorizing of its volume; Filtration obtains destainer, and destainer is concentrated into medicinal extract, and medicinal extract dissolves with 5% aqueous hydrochloric acid, filters; D151 Zeo-karb on the filtrating is washed till neutrality with deionized water earlier, uses the 85% ethanolic soln wash-out of 4LpH11 again, the elutriant concentrating under reduced pressure; Transfer pH10, place crystallization, filter and obtain crystallization, crystallization refluxes with acetone and dissolves; Filtered while hot is put cold crystallization, leaches crystallizing and drying and promptly gets product 153mg, and content is 88.2%.
Embodiment 2:
Get OX-heart sweetsop dry leave raw material 1kg, be crushed to 40 orders, add 500ml ammoniacal liquor ammonification 5 hours, add extraction kettle, adopt supercritical CO
2Extraction is an entrainment agent with methyl alcohol, and the volume percent that the entrainment agent consumption accounts for total extraction solvent is 5%, and extraction temperature is 50 ℃, and extracting pressure is 35MPa, and the separating still temperature is 35 ℃, and pressure is 6MPa, CO
2Flow is 3ml/g raw material/min, extracts 2 hours, resolves and to obtain extraction liquid, adds 1% activated carbon decolorizing of its volume; Filtration obtains destainer, and destainer is concentrated into medicinal extract, and medicinal extract dissolves with 5% aqueous sulfuric acid, filters; HZD-2 Zeo-karb on the filtrating is washed till neutrality with deionized water earlier, uses the 85% ethanolic soln wash-out of 5LpH9 again, the elutriant concentrating under reduced pressure; Transfer pH10, place crystallization, filter and obtain crystallization, crystallization refluxes with acetone and dissolves; Filtered while hot is put cold crystallization, leaches crystallizing and drying and promptly gets product 127mg, and content is 89.4%.
Embodiment 3:
Get OX-heart sweetsop dry leave raw material 5kg, be crushed to 30 orders, add 500ml ammoniacal liquor ammonification 4 hours, add extraction kettle, adopt supercritical CO
2Extraction is an entrainment agent with methyl alcohol, and the volume percent that the entrainment agent consumption accounts for total extraction solvent is 3%, and extraction temperature is 55 ℃, and extracting pressure is 35MPa, and the separating still temperature is 35 ℃, and pressure is 6MPa, CO
2Flow is 4ml/g raw material/min, extracts 3 hours, resolves and to obtain extraction liquid, adds 1% activated carbon decolorizing of its volume; Filtration obtains destainer, and destainer is concentrated into medicinal extract, and medicinal extract dissolves with 3% aqueous sulfuric acid, filters; HD-8 Zeo-karb on the filtrating is washed till neutrality with deionized water earlier, uses the 90% ethanolic soln wash-out of 25LpH10 again, the elutriant concentrating under reduced pressure; Transfer pH10, place crystallization, filter and obtain crystallization, crystallization refluxes with acetone and dissolves; Filtered while hot is put cold crystallization, leaches crystallizing and drying and promptly gets product 696mg, and content is 85.1%.
Embodiment 4:
Get OX-heart sweetsop dry leave raw material 5kg, be crushed to 40 orders, add 500ml ammoniacal liquor ammonification 2 hours, add extraction kettle, adopt supercritical CO
2Extraction is an entrainment agent with methyl alcohol, and the volume percent that the entrainment agent consumption accounts for total extraction solvent is 3%, and extraction temperature is 50 ℃, and extracting pressure is 30MPa, and the separating still temperature is 35 ℃, and pressure is 4MPa, CO
2Flow is 2ml/g raw material/min, extracts 4 hours, resolves and to obtain extraction liquid, adds 1% activated carbon decolorizing of its volume; Filtration obtains destainer, and destainer is concentrated into medicinal extract, and medicinal extract dissolves with 4% aqueous hydrochloric acid, filters; D151 Zeo-karb on the filtrating is washed till neutrality with deionized water earlier, uses the 90% ethanolic soln wash-out of 30LpH11 again, the elutriant concentrating under reduced pressure; Transfer pH10, place crystallization, filter and obtain crystallization, crystallization refluxes with acetone and dissolves; Filtered while hot is put cold crystallization, leaches crystallizing and drying and promptly gets product 584mg, and content is 91.3%.
Embodiment 5:
Get OX-heart sweetsop dry leave raw material 10kg, be crushed to 20 orders, add 4L ammoniacal liquor ammonification 6 hours, add extraction kettle, adopt supercritical CO
2Extraction is an entrainment agent with methyl alcohol, and the volume percent that the entrainment agent consumption accounts for total extraction solvent is 6%, and extraction temperature is 60 ℃, and extracting pressure is 38MPa, and the separating still temperature is 45 ℃, and pressure is 8MPa, CO
2Flow is 5ml/g raw material/min, extracts 4 hours, resolves and to obtain extraction liquid, adds 1% activated carbon decolorizing of its volume; Filtration obtains destainer, and destainer is concentrated into medicinal extract, and medicinal extract dissolves with 3% aqueous hydrochloric acid, filters; HD-8 Zeo-karb on the filtrating is washed till neutrality with deionized water earlier, uses the 75% ethanolic soln wash-out of 45LpH9 again, the elutriant concentrating under reduced pressure; Transfer pH11, place crystallization, filter and obtain crystallization, crystallization refluxes with acetone and dissolves; Filtered while hot is put cold crystallization, leaches crystallizing and drying and promptly gets product 1.2g, and content is 88.6%.
Claims (5)
1. the process for extracting of Ah's sago lobine is characterized in that may further comprise the steps:
(1) getting OX-heart sweetsop dry leave is raw material, is crushed to the 20-40 order, ammonification 2-6 hour, add extraction kettle, and adopt supercritical CO
2Extraction is an entrainment agent with methyl alcohol, extracts 2-4 hour, resolves and obtains extraction liquid;
(2) above-mentioned extraction liquid adds the activated carbon decolorizing of the 0.8-1% of its volume, filters and obtains destainer, and destainer is concentrated into medicinal extract;
(3) above-mentioned medicinal extract dissolves with sour water, filters, and Zeo-karb on the filtrating is washed till neutrality with deionized water earlier, uses the alkaline alcohol solution wash-out again, and the elutriant concentrating under reduced pressure is transferred pH10-11, places crystallization, filters and obtains crystallization;
(4) above-mentioned crystallization refluxes with acetone and dissolves, and filtered while hot is put cold crystallization, leaches crystallizing and drying and promptly gets product.
2. according to the process for extracting of the said a kind of Ah's sago lobine of claim 1, it is characterized in that supercritical CO in the said step (1)
2Extraction temperature is 50-60 ℃, and extracting pressure is 30-38MPa, and the separating still temperature is 30-45 ℃, and pressure is 4-8MPa, CO
2Flow is 2-5ml/g raw material/min, and the volume percent that the entrainment agent consumption accounts for total extraction solvent is 3-6%.
3. according to the process for extracting of the said a kind of Ah's sago lobine of claim 1, it is characterized in that sour water is hydrochloric acid or the aqueous sulfuric acid of 3-5% in the said step (3).
4. according to the process for extracting of the said a kind of Ah's sago lobine of claim 1, it is characterized in that in the said step (3) a kind of among the optional D151 of Zeo-karb, HZD-2 or the HD-8.
5. according to the process for extracting of the said a kind of Ah's sago lobine of claim 1, it is characterized in that said step (3) neutral and alkali alcoholic solution is the ethanolic soln of pH9-11, concentration is 75-90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103037019A CN102503889A (en) | 2011-10-10 | 2011-10-10 | Method for extracting asimilobine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103037019A CN102503889A (en) | 2011-10-10 | 2011-10-10 | Method for extracting asimilobine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102503889A true CN102503889A (en) | 2012-06-20 |
Family
ID=46216039
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103037019A Pending CN102503889A (en) | 2011-10-10 | 2011-10-10 | Method for extracting asimilobine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102503889A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110123814A (en) * | 2019-05-23 | 2019-08-16 | 上海科技大学 | Application of the asimilobine as the selective agonist of seretonine receptor hypotype 2C |
| CN117160184A (en) * | 2023-08-17 | 2023-12-05 | 清远市富盈电子有限公司 | Processing device and processing method for VOCs (volatile organic compounds) during PCB production |
-
2011
- 2011-10-10 CN CN2011103037019A patent/CN102503889A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110123814A (en) * | 2019-05-23 | 2019-08-16 | 上海科技大学 | Application of the asimilobine as the selective agonist of seretonine receptor hypotype 2C |
| CN117160184A (en) * | 2023-08-17 | 2023-12-05 | 清远市富盈电子有限公司 | Processing device and processing method for VOCs (volatile organic compounds) during PCB production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101857531B (en) | Method for extracting magnolol and honokiol from magnolia bark | |
| CN101863950A (en) | Method for extracting tea saponin from oil tea cakes | |
| CN102942550B (en) | Method for extracting cyanidin from black bean peel | |
| CN104086365B (en) | A kind of method of being prepared by antierythrite production mother liquor recycling to mixing sugar alcohol product | |
| CN105061532A (en) | Production method for hesperidin | |
| CN102220387B (en) | Method for extracting and purifying resveratrol and emodin from fresh giant knotweed | |
| CN113896754A (en) | Industrial production method for extracting and purifying baicalin from scutellaria baicalensis | |
| CN102731593A (en) | Method for extracting rutin from tartary buckwheat | |
| CN102464602A (en) | Method for extracting 5-hydroxytryptophan | |
| CN104262251A (en) | Method for extracting huperzine A from serrate clubmoss herb | |
| CN104262425A (en) | Novel method for extracting rubusoside | |
| CN102746345A (en) | Industrialized production method of high content tea polyphenol | |
| CN112266362B (en) | Method for extracting tetrahydropyrimidine by combining aqueous two-phase extraction with ion exchange chromatography | |
| CN102503889A (en) | Method for extracting asimilobine | |
| CN101759731B (en) | Extraction method of linseed gum and secoisolariciresin-ol diglucoside | |
| CN102924419A (en) | Method for extracting fisetin from boxwood | |
| CN101973983A (en) | Method for extracting orientins from Chinese globeflower flowers | |
| CN106967030A (en) | A kind of extraction and purification process of dihydromyricetin | |
| CN103860626A (en) | Method for preparing total flavonoids in eucommia ulmoides leaves | |
| CN106810564A (en) | The method for separating eurycomanone is extracted in a kind of root from Tongkat Ali | |
| CN102311379A (en) | Method for preparing 1-deoxynojirimycin by membrane separation technology | |
| CN103772457A (en) | Method for preparing geniposidic acid in eucommia leaf | |
| CN102329209A (en) | Method for extracting emodin from giant knotweed rhizome | |
| CN105315253A (en) | Method for producing pesticide-residue-free black rice anthocyanidin with black rice bran | |
| CN108707149A (en) | A kind of extracting method of berberine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120620 |