CN102875443A - Method for extracting abrine - Google Patents
Method for extracting abrine Download PDFInfo
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- CN102875443A CN102875443A CN2012103824860A CN201210382486A CN102875443A CN 102875443 A CN102875443 A CN 102875443A CN 2012103824860 A CN2012103824860 A CN 2012103824860A CN 201210382486 A CN201210382486 A CN 201210382486A CN 102875443 A CN102875443 A CN 102875443A
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- abrine
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- 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
- Y02P20/141—Feedstock
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to an efficient and low-pollution method for extracting abrine. The method includes steps of smashing a raw material of canton love-pea vine to 20-80 meshes, adding the raw material to an extraction kettle, feeding liquid CO2 and entrainer to the extraction kettle, extracting the raw material for 30-60 minutes at the temperature of 40-50 DEG C under the pressure of 20-30 MPa and then performing resolving at the temperature of 40-60 DEG C under the pressure of 5-9 MPa to obtain an extractant; and dissolving the extractant by using acid water, filtering the extractant by using a nanofiltration membrane, concentrating a filtering liquid by using a reverse osmosis membrane, adjusting potential of hydrogen (PH) of a concentrated solution to 5-6, adding an ethanol solution for ethanol precipitation, filtering out the solutions to obtain a precipitate, dissolving the precipitate by using a 70%-99% methanol solution, and performing recrystallization for 2-3 times to obtain the abrine. By means of the method for extracting the abrine, the method is simple in operation, the purity of the obtained abrine is high, and the industrial amplification is easy to achieve.
Description
Technical field
The invention belongs to biological technical field, relate to a kind of method that extracts abrine, have more and relate to a kind of employing supercritical CO
2Extraction and membrane filtration technique combine and extract the method for abrine.
Background technology
Abrine (abrine) be again Abrine, N-methyl-tryptophane, molecular formula C
12H
14N
2O
2, molecular weight 218.25, structural formula:
。
The high purity abrine is prism-shaped crystallization (water), 295 ℃ of decomposition points, specific rotation+44 ° (0.28g is dissolved in the 10m1 0.5mol/L hydrochloric acid).1g is dissolved in about 100ml methyl alcohol, is slightly soluble in water, is insoluble to ether, is dissolved in rare bronsted lowry acids and bases bronsted lowry.
Abrine is present in the seed of leguminous plants Semen Abri Precatorii, in the plants such as herb of Guangdong Semen Abri Precatorii (A. fruticulosus Wall.ex Wight et Arn.).Find that in pharmacological research abrine can obviously suppress mice auricle swelling, reduce Mice Auricle weight; Increase immune mouse thymus gland, spleen weight, improve the mice serum hemolysin level; Obviously reduce due to CCL4 and the α-naphthyl isothiocyanate transaminase activity and content of bilirubin in the liver injury mice serum, the protection liver injury.Also being found has restraining effect to the guinea pig experimental asthma reaction, and anaphylactic shock guinea-pigs is had provide protection, can suppress histamine phosphate and cause the increase of rat skin vascular permeability.
The method of existing extraction abrine generally adopts normal pressure to extract, and adopts silicagel column, gel column or preparation liquid phase process to separate again.Such as document " microwave-assisted extraction-efficient liquid phase chromatographic analysis prepares the research of abrine and Hypaphorine in the Herba Abri ".But the normal pressure extraction method exists extraction efficiency low, the shortcomings such as subsequent purification process operations complexity.
Summary of the invention
The objective of the invention is to overcome defective and the deficiency of prior art, a kind of method efficient, easy and simple to handle that extracts abrine is provided.
The objective of the invention is to be achieved through the following technical solutions:
1) Herba Abri raw material pulverizing 20-80 order drops into extraction kettle, passes into liquid CO
2And entrainment agent, under pressure 20-30MPa, temperature 40-55 ℃ condition, extraction 30-60min resolves under pressure 5-9MPa, temperature 40-60 ℃ condition, gets extract;
2) above-mentioned extract dissolves with sour water, filters with nanofiltration membrane, and filtrate is concentrated with reverse osmosis membrane again, and concentrated solution is regulated pH5-6 and added the ethanolic soln alcohol precipitation, leaches to get throw out 70-99% dissolve with methanol solution recrystallization 2-3 time, namely gets abrine.
Entrainment agent described in the step 1) is the 50-99% methanol solution, and consumption is 1-3 times of material quantity.
Step 2) nanofiltration membrane described in is the hollow cellulose film of molecular weight cut-off 400-1000.
Advantage of the present invention is:
A technology utilization supercritical CO
2Extraction, extraction efficiency is high, and stripping impurity is few, and environmentally friendly;
B process using membrane separation technique is a kind of physical separating process, and is simple to operate, and environmental protection, less energy-consumption.
Embodiment:
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
Herba Abri is pulverized 60 orders, takes by weighing 1kg and drops into extraction kettle, passes into liquid CO
2, regulate pressure 25MPa, temperature 50 C, reach above-mentioned parameter, pass into again 90% methanol solution, extraction 40min resolves extract under pressure 6MPa, 55 ℃ of conditions of temperature.The gained extract dissolves with the aqueous hydrochloric acid of pH3, hollow cellulose film nanofiltration with molecular weight cut-off 400, filtrate is concentrated with reverse osmosis membrane again, concentrated solution is regulated pH6 and is added the ethanolic soln alcohol precipitation, leach throw out with 85% dissolve with methanol solution recrystallization 3 times, the dry abrine 860mg that gets detects content 98.5% through HPLC.
Embodiment 2:
Herba Abri is pulverized 80 orders, takes by weighing 1kg and drops into extraction kettle, passes into liquid CO
2, regulate pressure 27MPa, temperature 45 C, reach above-mentioned parameter, pass into again 80% methanol solution, extraction 50min resolves extract under pressure 5MPa, temperature 60 C condition.The gained extract dissolves with the aqueous sulfuric acid of pH2, hollow cellulose film nanofiltration with molecular weight cut-off 500, filtrate is concentrated with reverse osmosis membrane again, concentrated solution is regulated pH5 and is added the ethanolic soln alcohol precipitation, leach throw out with 90% dissolve with methanol solution recrystallization 2 times, the dry abrine 920mg that gets detects content 97.8% through HPLC.
Embodiment 3:
Herba Abri is pulverized 40 orders, takes by weighing 1kg and drops into extraction kettle, passes into liquid CO
2, regulate pressure 22MPa, temperature 45 C, reach above-mentioned parameter, pass into again 60% methanol solution, extraction 30min resolves extract under pressure 5MPa, temperature 60 C condition.The gained extract dissolves with the aqueous hydrochloric acid of pH3, hollow cellulose film nanofiltration with molecular weight cut-off 600, filtrate is concentrated with reverse osmosis membrane again, concentrated solution is regulated pH5.5 and is added the ethanolic soln alcohol precipitation, leach throw out with 70% dissolve with methanol solution recrystallization 3 times, the dry abrine 780mg that gets detects content 98.1% through HPLC.
Claims (3)
1. method that extracts abrine is characterized in that following steps:
1) Herba Abri raw material pulverizing 20-80 order drops into extraction kettle, passes into liquid CO
2And entrainment agent, under pressure 20-30MPa, temperature 40-55 ℃ condition, extraction 30-60min resolves under pressure 5-9MPa, temperature 40-60 ℃ condition, gets extract;
2) above-mentioned extract dissolves with sour water, filters with nanofiltration membrane, and filtrate is concentrated with reverse osmosis membrane again, and concentrated solution is regulated pH5-6 and added the ethanolic soln alcohol precipitation, leaches to get throw out 70-99% dissolve with methanol solution recrystallization 2-3 time, namely gets abrine.
2. the method for extraction abrine according to claim 1 is characterized in that the entrainment agent described in the step 1) is the 50-99% methanol solution, and consumption is 1-3 times of material quantity.
3. the method for extraction abrine according to claim 1 is characterized in that step 2) described in nanofiltration membrane be the hollow cellulose film of molecular weight cut-off 400-1000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103824860A CN102875443A (en) | 2012-10-11 | 2012-10-11 | Method for extracting abrine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103824860A CN102875443A (en) | 2012-10-11 | 2012-10-11 | Method for extracting abrine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102875443A true CN102875443A (en) | 2013-01-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103824860A Pending CN102875443A (en) | 2012-10-11 | 2012-10-11 | Method for extracting abrine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558733A (en) * | 2017-12-29 | 2018-09-21 | 广西汇智生产力促进中心有限公司 | The method for extracting Canton love-pea vine abrine |
-
2012
- 2012-10-11 CN CN2012103824860A patent/CN102875443A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558733A (en) * | 2017-12-29 | 2018-09-21 | 广西汇智生产力促进中心有限公司 | The method for extracting Canton love-pea vine abrine |
| CN108558733B (en) * | 2017-12-29 | 2021-09-03 | 广西汇智生产力促进中心有限公司 | Method for extracting abrine from abrus cantoniensis hance |
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| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130116 |