CN102180808A - Method for refining pseudo-ginseng root total amino acid by applying membrane separation technology - Google Patents
Method for refining pseudo-ginseng root total amino acid by applying membrane separation technology Download PDFInfo
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- CN102180808A CN102180808A CN2011100291499A CN201110029149A CN102180808A CN 102180808 A CN102180808 A CN 102180808A CN 2011100291499 A CN2011100291499 A CN 2011100291499A CN 201110029149 A CN201110029149 A CN 201110029149A CN 102180808 A CN102180808 A CN 102180808A
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Abstract
The invention relates to a method for refining pseudo-ginseng root total amino acid by applying a membrane separation technology, in particular to a method for refining pseudo-ginseng root total amino acid by using a microfiltration membrane and a nanofiltration membrane. The method comprises the following steps of: grinding pseudo-ginseng root leaves; adding water and extracting for 1-3 times; combining extracting solutions; adding a flocculating agent under the stirring action; removing precipitates; adding a clarifying solution into a microfiltration device for microfiltration; adding microfiltration fluid into a nanofiltration device for nanofiltration; recycling a solvent from permeate liquid to a small volume; adding ethanol for precipitating; refluxing, dissolving and crystalizing the precipitates with ethanol with the concentration of 50-70 percent for 2-4 times; and drying to obtain a product. The method has the advantages of easiness of operation, no loss of amino acid and easy amplification of process.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, especially relate to a kind of method of using microfiltration membrane and the refining total propylhomoserin of pseudo-ginseng of nanofiltration membrane.
Background technology:
Pseudo-ginseng, Panax notoginseng (Burk.) F.H.Chen has another name called Radix Notoginseng, pseudo-ginseng, mountain lacquer, invaluable, and the araliaceae ginseng plant is warm in nature, sweet, little hardship of distinguishing the flavor of.Function cures mainly: the stasis of blood of loosing hemostasis, subduing swelling and relieving pain.Be used for various inside and outside hemorrhage, chest ventral spine pain, tumbling and swelling.The Compendium of Material Medica record pseudo-ginseng flavor of genseng " quite like ", " analgesic therapy of styptic powder blood " can control all mass formed by blood stasis, goes through in edition Chinese Pharmacopoeia also function with pseudo-ginseng and cures mainly and be defined as hemostasis.Modern pharmacological research shows that the non-protein amino acid in the pseudo-ginseng has extraordinary haemostatic effect, is the main hemostatic compositions of pseudo-ginseng.
The total propylhomoserin of pseudo-ginseng, main component are dencichine (dencichine): molecular formula, C
5H
8N
2O
5Molecular weight, 176.13; Its semihydrate is colourless crystallization (50% ethanol), and is soluble in water, is insoluble to methyl alcohol, ethanol, propyl alcohol, acetone and other organic solvent.Zhang Yong etc. discover that the pseudo-ginseng intravenous injection has significantly preventative and curative anastalsis, and its main hemostatic mechanism is to shorten whole blood coagulation time, promotion blood coagulation, minimizing blood plasma TAP level and reduce fibrinolytic activity.Pseudo-ginseng now has been subjected to extensive attention as potent haemostatic medicament, and wide research prospect is arranged.
Existing dencichine mainly makes by synthesizing and extracting two aspects.The extraction of dencichine mainly is by first alcohol extracting, residue water is carried, after extracting solution concentrates again through n-butanol extraction, Sephadex LH-20 and CM Sephadex C-25 resin make on the raffinate layer, this method makes dencichine content height, but preparation amount is little, and the Sephadex LH-2 that uses and CM Sephadex C-25 price are comparatively expensive, cost is higher, is not suitable for a large amount of preparations.Existing patent " is extracted the method for dencichine " from the pseudo-ginseng (patent No.: 200610027962.1), the method that this patent adopts is first alcohol extracting, residue is then used flooding, use n-butanol extraction behind the extracting solution alcohol precipitation, resin cation (R.C.) on the raffinate, the elutriant acetone precipitation, last recrystallization obtains the higher dencichine of purity, and this method solvent load is big.
Summary of the invention:
1, goal of the invention: the object of the present invention is to provide a kind of method that is applicable to the total propylhomoserin of industrialization extraction pseudo-ginseng.
2, technical scheme:
The method of the refining total propylhomoserin of pseudo-ginseng of a kind of using membrane separating technology is characterized in that may further comprise the steps:
1) extracts: Sanchi Leaf is pulverized, added 5～12 times of water gagings and extract united extraction liquid 1～3 time;
2) removal of impurities: stir said extracted liquid, under stirring fast, slowly add flocculant solution, stir at a slow speed after mixing, leave standstill 2～8h, centrifugal or filter with precipitate and separate, clear liquor;
3) membrane sepn: above-mentioned clear liquor is added micro-filtration in the micro-filtration, and micro-filtrate adds nanofiltration in the nanofiltration device again, collects to see through liquid;
4) recrystallization: the above-mentioned liquid that sees through reclaims solvent to small volume, adds ethanol sedimentation, leaches throw out with 50～70% dissolve with ethanol crystallizations 2～4 times, is drying to obtain product.
Extracting mode in the step 1) can be selected a kind of in backflow, cold soaking, the supersound extraction for use.
Step 2) flocculation agent in is a CTS Chinese medicine flocculation agent, and consumption is 0.1 of soup～0.8 ‰; The preparation method of flocculant solution is, earlier flocculation agent is dissolved in water, and dilution is 1～2% flocculant solution.
Microfiltration membrane in the step 3) is selected inorganic ceramic film for use, and material is aluminum oxide, zirconium white, weisspiessglanz or titanium oxide, holds back particle range 100～200nm, and filtration pressure is 200～500kPa.
Nanofiltration membrane in the step 3) is selected organic hybrid films for use, and material is polyester, polyethylene kind or polyamide-based, and molecular weight cut-off is 200～400, and filtration pressure is 500～800kPa.
Crystallization condition in the step 4) is the dissolvings of 50～70% alcohol refluxs, and solution is recycled to 1/3～1/10 of original volume, leaves standstill crystallization.
Advantage of the present invention is the following aspects:
1. this process using membrane-membrane separates, and simple to operate, the extraction yield height has been removed most of impurity;
2. adopt inorganic ceramic film separation efficiency height, but cold operation, and the amino acid free of losses makes good product quality;
3. adopt the nanofiltration membrane impurity trapped, hold back arasaponin class, flavonoid impurity, nanofiltration sees through in the liquid and obtains micromolecular amino acid, and is simple to operate, lossless.
In sum, the present invention have the loss of mild condition, amino acid less, operation is few, advantages such as preparation amount is big, save energy are suitable for industrialization and amplify.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Sanchi Leaf is pulverized, take by weighing 1Kg, add the lixiviate of 12L water-cooled and get 2 times, filter, united extraction liquid, get 2.5gCTS Chinese medicine flocculation agent, add the dilution of 250ml water, extracting solution is adding the CTS diluent under the stirring action fast, stir at a slow speed after mixing, leave standstill 3h, remove by filter precipitation, filtrate adds micro-filtration in the alumina ceramic membrane, interception is 200nm, filtration pressure is 200kPa, nanofiltration in the polyester composite nanometer filtering film of collection micro-filtrate adding molecular retention amount 400, and filtration pressure is 500kPa, collect and see through liquid, reclaim solvent to small volume, add ethanol sedimentation, leach throw out with 50% ethanolic soln heating for dissolving, be concentrated into 1/3 volume, leave standstill crystallization 2 times, drying obtains white solid 8.1g, contains dencichine 72.2%.
Embodiment 2:
Sanchi Leaf is pulverized, take by weighing 1Kg, add 5L water refluxing extraction 2 times, filter, united extraction liquid, get 6gCTS Chinese medicine flocculation agent, add the dilution of 300ml water, extracting solution is adding the CTS diluent under the stirring action fast, stir at a slow speed after mixing, leave standstill 5h, the centrifugal precipitation of removing, centrifugate adds micro-filtration in the titanium oxide ceramics film, interception is 100nm, filtration pressure is 500kPa, nanofiltration in the polyethylene kind composite nanometer filtering film of collection micro-filtrate adding molecular retention amount 300, and filtration pressure is 600kPa, collect and see through liquid, reclaim solvent to small volume, add ethanol sedimentation, leach throw out with 60% ethanolic soln heating for dissolving, be concentrated into 1/4 volume, leave standstill crystallization 3 times, drying obtains white solid 7.3g, contains dencichine 74.9%.
Embodiment 3:
Sanchi Leaf is pulverized, take by weighing 1Kg, add 6L water supersound extraction 2 times, filter, united extraction liquid, get 4gCTS Chinese medicine flocculation agent, add the dilution of 300ml water, extracting solution is adding the CTS diluent under the stirring action fast, stir at a slow speed after mixing, leave standstill 6h, remove by filter precipitation, filtrate adds micro-filtration in the zirconia ceramics film, interception is 200nm, filtration pressure is 300kPa, nanofiltration in the polyamide-based composite nanometer filtering film of collection micro-filtrate adding molecular retention amount 200, and filtration pressure is 800kPa, collect and see through liquid, reclaim solvent to small volume, add ethanol sedimentation, leach throw out with 65% ethanolic soln heating for dissolving, be concentrated into 1/5 volume, leave standstill crystallization 2 times, drying obtains white solid 8.7g, contains dencichine 68.4%.
Embodiment 4:
Sanchi Leaf is pulverized, take by weighing 5Kg, add 40L water refluxing extraction 2 times, filter, united extraction liquid, get 15gCTS Chinese medicine flocculation agent, add the dilution of 1L water, extracting solution is adding the CTS diluent under the stirring action fast, stir at a slow speed after mixing, leave standstill 4h, the centrifugal precipitation of removing, centrifugate adds micro-filtration in the alumina ceramic membrane, interception is 300nm, filtration pressure is 250kPa, nanofiltration in the polyester composite nanometer filtering film of collection micro-filtrate adding molecular retention amount 300, and filtration pressure is 650kPa, collect and see through liquid, reclaim solvent to small volume, add ethanol sedimentation, leach throw out with 70% ethanolic soln heating for dissolving, be concentrated into 1/10 volume, leave standstill crystallization 4 times, drying obtains white solid 38.2g, contains dencichine 69.2%.
Embodiment 5:
Sanchi Leaf is pulverized, take by weighing 5Kg, add 30L water supersound extraction 3 times, filter, united extraction liquid, get 20gCTS Chinese medicine flocculation agent, add the dilution of 3L water, extracting solution is adding the CTS diluent under the stirring action fast, stir at a slow speed after mixing, leave standstill 5h, remove by filter precipitation, filtrate adds micro-filtration in the weisspiessglanz ceramic membrane, interception is 400nm, filtration pressure is 350kPa, nanofiltration in the polyester composite nanometer filtering film of collection micro-filtrate adding molecular retention amount 400, and filtration pressure is 700kPa, collect and see through liquid, reclaim solvent to small volume, add ethanol sedimentation, leach throw out with 55% ethanolic soln heating for dissolving, be concentrated into 1/8 volume, leave standstill crystallization 2 times, drying obtains white solid 42.1g, contains dencichine 73.8%.
Embodiment 6:
Sanchi Leaf is pulverized, take by weighing 10Kg, add 50L water refluxing extraction 2 times, filter, united extraction liquid, get 45gCTS Chinese medicine flocculation agent, add the dilution of 8L water, extracting solution is adding the CTS diluent under the stirring action fast, stir at a slow speed after mixing, leave standstill 6h, the centrifugal precipitation of removing, centrifugate adds micro-filtration in the titanium oxide ceramics film, interception is 300nm, filtration pressure is 400kPa, nanofiltration in the polyester composite nanometer filtering film of collection micro-filtrate adding molecular retention amount 300, and filtration pressure is 650kPa, collect and see through liquid, reclaim solvent to small volume, add ethanol sedimentation, leach throw out with 70% ethanolic soln heating for dissolving, be concentrated into 1/7 volume, leave standstill crystallization 3 times, drying obtains white solid 71.7g, contains dencichine 75.3%.
Claims (6)
1. the method for the refining total propylhomoserin of pseudo-ginseng of a using membrane separating technology is characterized in that comprising following steps:
1) extracts: Sanchi Leaf is pulverized, added 5～12 times of water gagings and extract united extraction liquid 1～3 time;
2) removal of impurities: stir said extracted liquid, under stirring fast, slowly add flocculant solution, stir at a slow speed after mixing, leave standstill 2～8h, centrifugal or filter with precipitate and separate, clear liquor;
3) membrane sepn: above-mentioned clear liquor is added micro-filtration in the micro-filtration, and micro-filtrate adds nanofiltration in the nanofiltration device again, collects to see through liquid;
4) recrystallization: the above-mentioned liquid that sees through reclaims solvent to small volume, adds ethanol sedimentation, leaches throw out with 50～70% dissolve with ethanol crystallizations 2～4 times, is drying to obtain product.
2. the method for the refining total propylhomoserin of pseudo-ginseng of a kind of using membrane separating technology as claimed in claim 1 is characterized in that extracting mode in the described step 1) can select a kind of in backflow, cold soaking, the supersound extraction for use.
3. the method for the refining total propylhomoserin of pseudo-ginseng of a kind of using membrane separating technology as claimed in claim 1 is characterized in that described step 2) in flocculation agent be CTS Chinese medicine flocculation agent, consumption is 0.1 of soup～0.8 ‰; The preparation method of flocculant solution is: earlier flocculation agent is dissolved in water, dilution is 1～2% flocculant solution.
4. the method for the refining total propylhomoserin of pseudo-ginseng of a kind of using membrane separating technology as claimed in claim 1, it is characterized in that the microfiltration membrane in the described step 3) selects inorganic ceramic film for use, material is aluminum oxide, zirconium white, weisspiessglanz or titanium oxide, hold back particle range 100～200nm, filtration pressure is 200～500kPa.
5. the method for the refining total propylhomoserin of pseudo-ginseng of a kind of using membrane separating technology as claimed in claim 1, it is characterized in that the nanofiltration membrane in the described step 3) selects organic hybrid films for use, material is polyester, polyethylene kind or polyamide-based, molecular weight cut-off is 200～400, and filtration pressure is 500～800kPa.
6. the method for the refining total propylhomoserin of pseudo-ginseng of a kind of using membrane separating technology as claimed in claim 1 is characterized in that the crystallization condition in the described step 4) is the dissolvings of 50～70% alcohol refluxs, and solution is recycled to 1/3～1/10 of original volume, leaves standstill crystallization.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103735634A (en) * | 2014-01-08 | 2014-04-23 | 广州发元生物科技有限公司 | Black hair-nourishing traditional Chinese medicine composition and preparation method thereof |
| CN107824049A (en) * | 2017-11-13 | 2018-03-23 | 安徽名创新材料科技有限公司 | A kind of method of shearing technique strengthening the membrane separation process |
| CN113214081A (en) * | 2021-03-19 | 2021-08-06 | 南阳理工学院 | Method for flocculating, decoloring and purifying rosmarinic acid by membrane separation |
| CN117417006A (en) * | 2023-11-23 | 2024-01-19 | 青岛百发海水淡化有限公司 | Seawater desalination pretreatment process system in low-temperature state and operation method |
-
2011
- 2011-01-24 CN CN2011100291499A patent/CN102180808A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103735634A (en) * | 2014-01-08 | 2014-04-23 | 广州发元生物科技有限公司 | Black hair-nourishing traditional Chinese medicine composition and preparation method thereof |
| CN103735634B (en) * | 2014-01-08 | 2016-01-06 | 广州发元生物科技有限公司 | There is Chinese medicine composition of blackening and nourishing hair effect and preparation method thereof |
| CN107824049A (en) * | 2017-11-13 | 2018-03-23 | 安徽名创新材料科技有限公司 | A kind of method of shearing technique strengthening the membrane separation process |
| CN113214081A (en) * | 2021-03-19 | 2021-08-06 | 南阳理工学院 | Method for flocculating, decoloring and purifying rosmarinic acid by membrane separation |
| CN113214081B (en) * | 2021-03-19 | 2024-04-09 | 南阳理工学院 | Flocculation decolorization and membrane separation method for purifying rosmarinic acid |
| CN117417006A (en) * | 2023-11-23 | 2024-01-19 | 青岛百发海水淡化有限公司 | Seawater desalination pretreatment process system in low-temperature state and operation method |
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Application publication date: 20110914 |