CN102286031A - Method for extracting and purifying corilagin - Google Patents
Method for extracting and purifying corilagin Download PDFInfo
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- CN102286031A CN102286031A CN2011101879050A CN201110187905A CN102286031A CN 102286031 A CN102286031 A CN 102286031A CN 2011101879050 A CN2011101879050 A CN 2011101879050A CN 201110187905 A CN201110187905 A CN 201110187905A CN 102286031 A CN102286031 A CN 102286031A
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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
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- 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
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Abstract
The invention relates to a method for extracting and purifying corilagin, which comprises: subjecting common leafflower herb to absorption by macroporous resin and desorption from macroporous resin; extracting concentrated desorption solution with n-butyl alcohol; concentrating the extraction solution, extracting corilagin extraction solution by using supercritical carbon dioxide fluid; further purifying the extraction solution by gel column chromatography; and recrystallizing to obtain corilagin. Compared with the prior art, the preparation method is simple in operation, low in cost and suitable for industrial production.
Description
Technical field
The invention belongs to the Chemistry for Chinese Traditional Medicine field, relate to a kind of method of extracting the purifying corilagin, specifically, relate to a kind of technology such as macroporous resin, supercritical carbon dioxide extraction and gel filtration chromatography that adopt in conjunction with the method for from Common Leafflower Herb, extracting the purifying corilagin.
Background technology
Corilagin is a kind of ellagic tannin, mainly is present in the plants such as close mandarin orange grass, Common Leafflower Herb, Herba Erodii molecular formula: C
27H
22O
18Molecular weight: 634.453, white needle powder is soluble in methyl alcohol, ethanol, Aceton, DMSO, and solubleness is little in cold water.Traditional natural drug is used history prompting corilagin has the better prevention effect to chronic cardiovascular disease, studies show that in recent years, corilagin has certain effect at aspects such as control blood coagulation, thrombosis, hypertension and atherosclerosiss, in addition, corilagin has restraining effect to some tumour and virus, and toxicity is also very low.
Common Leafflower Herb has another name called Herba Phyllanthi Urinariae, is the euphorbia plant Common Leafflower Herb
Phyllanthus UrinariaL. dry herb, effect with the flat liver of heat-clearing, convergence Li Shui, detoxify and promote the subsdence of swelling, among the peoplely be usually used in treating diseases such as diarrhoea, diarrhea, urinary tract infections, nephritic edema and icterohepatitis, its chemical ingredients is mainly multiple compounds such as flavonoid, Polyphenols, lignanoids, alkaloids.Its Polyphenols composition is its main active ingredient, have thrombolysis as Polyphenols compositions such as corilagin corilagin, gallic acid, ellagic acids, suppress thrombosis, hypertension and antiatherogenic effect, the spasmolysis and analgesia effect, effects such as anti-bacteria and anti-virus.
The extracting method of corilagin mainly adopts alcohol extracting or acetone extraction, and purification process mainly adopts methods such as ZTC resin column chromatography, organic solvent extraction.Chinese patent (application number 201010535378.3) " a kind of preparation method of corilagin " disclosed method is to adopt supercritical CO
2Technology such as extraction, macroporous resin adsorption and counter-current extraction are in conjunction with obtaining corilagin, and this method cost height, selectivity height, to put forward rate low.
Summary of the invention
The object of the present invention is to provide a kind of is raw material with the Common Leafflower Herb, by water carry, macroporous adsorption resin technology, supercritical liquid extraction technique, gel filtration chromatography technology and recrystallization technology combine, and obtains the processing method of high purity corilagin fast.
The objective of the invention is to be achieved through the following technical solutions:
Get the Common Leafflower Herb pulverizing medicinal materials, extract under 80-100 ℃ of condition with 8-15 pure water doubly, with extracting solution 65%-80% methanol aqueous solution wash-out after macroporous resin adsorption, elutriant is evaporated to small volume, the concentrated solution n-butanol extraction, extraction liquid is used supercritical CO after concentrating
2The extraction corilagin separates by gel filtration chromatography again, with 45%-60% acetone soln wash-out, collects elutriant, and concentrating under reduced pressure leaves standstill crystallization, and recrystallization promptly.
Macroporous adsorbent resin adopts D101, ADS-5, H1020, LAS-7 or D130 type macroporous adsorbent resin.
Supercritical CO
2Extraction conditions is: extracting pressure 20-28MPa, and extraction temperature 30-55 ℃, extraction time 2-6h resolves pressure 5-8MPa, and temperature 28-40 ℃, CO
2Flow velocity is 20-25L/h, the optional acetone of entrainment agent, ethanolic soln, and preferred acetone soln, volume percent is 50-70%, add-on is the 10-20% of medicinal material amount.
Recrystallization solvent is that one or more solution in Virahol, propylene glycol, ether, ethanol, the methylene dichloride mix.
Advantage of the present invention is:
The present invention extracts earlier and uses macroporous adsorbent resin enrichment corilagin composition again, carries out supercritical extraction again, the extraction yield height, and impurity is few, gel filtration chromatography separation and purification, good product quality, purity height.
Embodiment
Embodiment 1:
Taking by weighing Common Leafflower Herb medicinal material 2kg drops in the extraction equipment, use the 18kg pure water, be heated to 90 ℃, stir and extracted 1 hour, after the filtration, add the 15kg pure water again and be heated to 90 ℃, stir and extracted 1 hour, filter, the D130 macroporous adsorptive resins absorption that the pre-treatment of twice filtrate merga pass is good, elder generation's water is eluted to colourless, use 70% methanol-eluted fractions again, collect elutriant, be evaporated to small volume, with the n-butanol extraction of concentrated solution with equal volume amounts, extraction liquid concentrates in the back input supercritical carbon dioxide extraction still, and dynamic continuous extraction is 3 hours under the condition of 38 ℃ of extraction temperature and extracting pressure 28MPa, resolves pressure 6MPa, 30 ℃ of temperature, CO
2Flow velocity is 22L/h, entrainment agent is 60% acetone soln, and add-on is 15% of a medicinal material amount, collects faint yellow paste corilagin, Toyopearl HW-40 post will be gone up after the gained medicinal extract water dissolution, with 55% acetone soln wash-out, elutriant reclaims acetone, concentrates, leave standstill crystallization, the ether recrystallization gets the 2.39g corilagin, detects through HPLC, and its content is 98.3%.
Embodiment 2:
Taking by weighing Common Leafflower Herb medicinal material 2kg drops in the extraction equipment, use the 26kg pure water, be heated to 85 ℃, stir and extracted 1.5 hours, after the filtration, add the 20kg pure water again and be heated to 85 ℃, stir and extracted 1 hour, filter, the ADS-5 macroporous adsorptive resins absorption that the pre-treatment of twice filtrate merga pass is good, elder generation's water is eluted to colourless, use 80% methanol-eluted fractions again, collect elutriant, be evaporated to small volume, with the n-butanol extraction of concentrated solution with equal volume amounts, extraction liquid concentrates in the back input supercritical carbon dioxide extraction still, and dynamic continuous extraction is 5 hours under the condition of 42 ℃ of extraction temperature and extracting pressure 21.5MPa, resolves pressure 7MPa, 36 ℃ of temperature, CO
2Flow velocity is 20L/h, entrainment agent is 50% ethanolic soln, and add-on is 20% of a medicinal material amount, collects faint yellow paste corilagin, MCl-gel CHP-20P post will be gone up after the gained medicinal extract water dissolution, with 50% acetone soln wash-out, elutriant reclaims acetone, concentrates, leave standstill crystallization, ethyl alcohol recrystallization gets the 2.46g corilagin, detects through HPLC, and its content is 98.6%.
Embodiment 3:
Taking by weighing Common Leafflower Herb medicinal material 2kg drops in the extraction equipment, use the 30kg pure water, be heated to 100 ℃, stir and extracted 2 hours, after the filtration, add the 25kg pure water again and be heated to 100 ℃, stir and extracted 2 hours, filter, the D101 macroporous adsorptive resins absorption that the pre-treatment of twice filtrate merga pass is good, elder generation's water is eluted to colourless, use 65% methanol-eluted fractions again, collect elutriant, be evaporated to small volume, with the n-butanol extraction of concentrated solution with equal volume amounts, extraction liquid concentrates in the back input supercritical carbon dioxide extraction still, and dynamic continuous extraction is 2 hours under the condition of 31 ℃ of extraction temperature and extracting pressure 23MPa, resolves pressure 5MPa, 28 ℃ of temperature, CO
2Flow velocity is 25L/h, entrainment agent is 70% acetone soln, and add-on is 13% of a medicinal material amount, collects faint yellow paste corilagin, Toyopearl HW-40 post will be gone up after the gained medicinal extract water dissolution, with 45% acetone soln wash-out, elutriant reclaims acetone, concentrates, leave standstill crystallization, the propylene glycol recrystallization gets the 2.38g corilagin, detects through HPLC, and its content is 98.5%.
Embodiment 4:
Taking by weighing Common Leafflower Herb medicinal material 2kg drops in the extraction equipment, use the 20kg pure water, be heated to 80 ℃, stir and extracted 1 hour, after the filtration, add the 15kg pure water again and be heated to 80 ℃, stir and extracted 0.5 hour, filter, the LAS-7 macroporous adsorptive resins absorption that the pre-treatment of twice filtrate merga pass is good, elder generation's water is eluted to colourless, use 75% methanol-eluted fractions again, collect elutriant, be evaporated to small volume, with the n-butanol extraction of concentrated solution with equal volume amounts, extraction liquid concentrates in the back input supercritical carbon dioxide extraction still, and dynamic continuous extraction is 6 hours under the condition of 50 ℃ of extraction temperature and extracting pressure 24.8MPa, resolves pressure 8MPa, 35 ℃ of temperature, CO
2Flow velocity is 23L/h, entrainment agent is 65% ethanolic soln, and add-on is 10% of a medicinal material amount, collects faint yellow paste corilagin, MCl-gel CHP-20P post will be gone up after the gained medicinal extract water dissolution, with 60% acetone soln wash-out, elutriant reclaims acetone, concentrates, leave standstill crystallization, methylene dichloride-Virahol recrystallization gets the 2.49g corilagin, detects through HPLC, and its content is 98.0%.
Embodiment 5:
Taking by weighing Common Leafflower Herb medicinal material 2kg drops in the extraction equipment, use the 16kg pure water, be heated to 95 ℃, stir and extracted 2.5 hours, after the filtration, add the 13kg pure water again and be heated to 95 ℃, stir and extracted 2 hours, filter, the H1020 macroporous adsorptive resins absorption that the pre-treatment of twice filtrate merga pass is good, elder generation's water is eluted to colourless, use 80% methanol-eluted fractions again, collect elutriant, be evaporated to small volume, with the n-butanol extraction of concentrated solution with equal volume amounts, extraction liquid concentrates in the back input supercritical carbon dioxide extraction still, and dynamic continuous extraction is 4 hours under the condition of 53 ℃ of extraction temperature and extracting pressure 20.5MPa, resolves pressure 5.5MPa, 40 ℃ of temperature, CO
2Flow velocity is 24L/h, entrainment agent is 55% acetone soln, and add-on is 17% of a medicinal material amount, collects faint yellow paste corilagin, Sephadex LH-20 post will be gone up after the gained medicinal extract water dissolution, with 50% acetone soln wash-out, elutriant reclaims acetone, concentrates, leave standstill crystallization, the methylene dichloride recrystallization gets the 2.17g corilagin, detects through HPLC, and its content is 98.8%.
Claims (4)
1. method of extracting the purifying corilagin, it is characterized in that may further comprise the steps: get the Common Leafflower Herb pulverizing medicinal materials, extract under 80-100 ℃ of condition with 8-15 pure water doubly, with extracting solution 65%-80% methanol aqueous solution wash-out after macroporous resin adsorption, elutriant is evaporated to small volume, the concentrated solution n-butanol extraction, extraction liquid is used supercritical CO after concentrating
2The extraction corilagin separates by gel filtration chromatography again, with 45%-60% acetone soln wash-out, collects elutriant, and concentrating under reduced pressure leaves standstill crystallization, and recrystallization promptly.
2. a kind of method of extracting the purifying corilagin as claimed in claim 1 is characterized in that macroporous adsorbent resin adopts D101, ADS-5, H1020, LAS-7 or D130 type macroporous adsorbent resin.
3. a kind of method of extracting the purifying corilagin as claimed in claim 1 is characterized in that supercritical CO
2Extraction conditions is: extracting pressure 20-28MPa, and extraction temperature 30-55 ℃, extraction time 2-6h resolves pressure 5-8MPa, and temperature 28-40 ℃, CO
2Flow velocity is 20-25L/h, the optional acetone of entrainment agent, ethanolic soln, and preferred acetone soln, volume percent is 50-70%, add-on is the 10-20% of medicinal material amount.
4. a kind of method of extracting the purifying corilagin as claimed in claim 1 is characterized in that recrystallization solvent is one or more solution mixing in Virahol, propylene glycol, ether, ethanol, the methylene dichloride.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101879050A CN102286031A (en) | 2011-07-06 | 2011-07-06 | Method for extracting and purifying corilagin |
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|---|---|---|---|
| CN2011101879050A CN102286031A (en) | 2011-07-06 | 2011-07-06 | Method for extracting and purifying corilagin |
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| CN102286031A true CN102286031A (en) | 2011-12-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447896A (en) * | 2014-11-12 | 2015-03-25 | 广东食品药品职业学院 | Extraction-separation method and application of corilagin |
| CN105061522A (en) * | 2015-08-14 | 2015-11-18 | 厦门华侨亚热带植物引种园 | Preparation method of beta-1-O-galloyl-3, 6-(R)-hexahydroxy diphenoyl-D-glucose |
| CN109674804A (en) * | 2019-02-02 | 2019-04-26 | 武汉大学 | Corilagin is preparing the purposes in resisting myocardial fibrillation drug |
| CN111269277A (en) * | 2020-04-07 | 2020-06-12 | 云南农业大学 | Method for extracting and separating isochrysotium from garden burnet |
| CN114591381A (en) * | 2022-03-23 | 2022-06-07 | 集美大学 | Method for extracting corilagin from fructus Phyllanthi and application thereof |
-
2011
- 2011-07-06 CN CN2011101879050A patent/CN102286031A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447896A (en) * | 2014-11-12 | 2015-03-25 | 广东食品药品职业学院 | Extraction-separation method and application of corilagin |
| CN104447896B (en) * | 2014-11-12 | 2017-04-19 | 广东食品药品职业学院 | Extraction-separation method and application of corilagin |
| CN105061522A (en) * | 2015-08-14 | 2015-11-18 | 厦门华侨亚热带植物引种园 | Preparation method of beta-1-O-galloyl-3, 6-(R)-hexahydroxy diphenoyl-D-glucose |
| CN109674804A (en) * | 2019-02-02 | 2019-04-26 | 武汉大学 | Corilagin is preparing the purposes in resisting myocardial fibrillation drug |
| CN109674804B (en) * | 2019-02-02 | 2021-04-16 | 武汉大学 | Application of corilagin in preparation of anti-myocardial fibrosis drugs |
| CN111269277A (en) * | 2020-04-07 | 2020-06-12 | 云南农业大学 | Method for extracting and separating isochrysotium from garden burnet |
| CN114591381A (en) * | 2022-03-23 | 2022-06-07 | 集美大学 | Method for extracting corilagin from fructus Phyllanthi and application thereof |
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Application publication date: 20111221 |