CN104086537A - Method for extracting justicidin A from creeping rostellularia herb - Google Patents
Method for extracting justicidin A from creeping rostellularia herb Download PDFInfo
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- CN104086537A CN104086537A CN201410266261.8A CN201410266261A CN104086537A CN 104086537 A CN104086537 A CN 104086537A CN 201410266261 A CN201410266261 A CN 201410266261A CN 104086537 A CN104086537 A CN 104086537A
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- justicidin
- concentrated solution
- extracting
- under reduced
- reduced pressure
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
Abstract
The invention discloses a method for extracting justicidin A from creeping rostellularia herbs. The method comprises the following steps: (1) smashing the creeping rostellularia herbs serving as a raw material, adding 80-95 percent ethanol in an amount of 7-10 times that of the creeping rostellularia herbs, performing reflux extraction twice, combining two extracting solutions, recovering the ethanol, adding a concentrated solution into macroporous resin for adsorbing, eluting with a 50-90 percent ethanol solution in a volume of 5-10 times of the column volume, collecting eluent, and concentrating under reduced pressure to obtain a concentrated solution; (2) adding ethyl acetate into the concentrated solution for extracting, continually concentrating extraction liquid into extract, separating by adopting high-speed counter-current chromatography, collecting fluid according to a chromatogram, and drying the fluid under reduced pressure to obtain the justicidin A. The method is simple in production process, has high operability, and is suitable for producing the high-purity justicidin A.
Description
Technical field
The invention belongs to biological technical field, particularly a kind of method of extracting justicidin A from justicia grass.
Background technology
Justicidin A belongs to lignanoids material, CAS 25001-57-4, and molecular formula C22H18O7, molecular weight 394.38, molecular structural formula:
Justicia grass is the herb of acanthaceous plant justicia, and clearing heat and detoxicating, dampness removing disappears stagnant, promoting blood circulation and stopping pain.The heating that cures cold, cough, laryngalgia, malaria, dysentery, jaundice, ephritis edema, arthralgia and myalgia, infantile malnutrition, ulcer furunculosis, wound., herb is containing lignans such as alkaloid, justicidin A.Justicidin A has antiviral and cytotoxic activity.
By literature search, the existing justicidin A for preparing adopts silicagel column to separate more, complicated operation, and yield is low, and production cost is high.
Summary of the invention
The object of the invention is to solve prior art deficiency and defect, a kind of method of extracting justicidin A from justicia grass easy and simple to handle is provided.
The object of the present invention is achieved like this: a kind of method of extracting justicidin A from justicia grass, is characterized in that following steps:
1) by justicia grass raw material pulverizing, add 7-10 doubly to measure 80-95% alcohol reflux twice, merge extracted twice liquid and reclaim ethanol, concentrated solution adds in macroporous resin and adsorbs, with 5-10 times of column volume 50-90% ethanolic soln wash-out, collect elutriant concentrating under reduced pressure, obtain concentrated solution;
2) above-mentioned concentrated solution adds ethyl acetate extraction, extraction liquid to continue to be condensed into medicinal extract to adopt high speed adverse current chromatogram to separate, collect flow point according to collection of illustrative plates, flow point drying under reduced pressure and get final product.
The one of the optional AB-8 of described macroporous resin, ADS-21, HPD500 and NK-II in described step 1).
Described step 2) high speed adverse current chromatogram separation condition is: solvent systems selects ethyl acetate, propyl carbinol, water, and blending ratio 2-5:1-3:3-7 gets the phase that fixes mutually, the lower moving phase of doing mutually, engine speed 700-1000rpm, flow velocity 1-3ml/min
Adopt the present invention to prepare justicidin A, production technique is simple, and product purity is high, and production cost is low, is easy to realize suitability for industrialized production.
embodiment:
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment 1:
Get 5kg justicia grass raw material pulverizing, add 10 times of amount 95% alcohol reflux twice, merge extracted twice liquid and reclaim ethanol, concentrated solution dilute with water adds in AB-8 macroporous resin and adsorbs, with 8 times of column volumes, 70% ethanolic soln wash-out, collect elutriant concentrating under reduced pressure, concentrated solution is extracted with ethyl acetate, extraction liquid reclaims actual, obtains medicinal extract.Get ethyl acetate, propyl carbinol, water, 2:1:3 mixes in proportion, gets and injects mutually the chromatotube phase that fixes, engine speed 700rpm, take off and do mutually moving phase, flow velocity 2ml/min, collects flow point according to collection of illustrative plates, flow point drying under reduced pressure obtains justicidin A 2.3g, detects content 98.5% through HPLC.
Embodiment 2:
Get 5kg justicia grass raw material pulverizing, add 10 times of amount 80% alcohol reflux twice, merge extracted twice liquid and reclaim ethanol, concentrated solution dilute with water adds in ADS-21 macroporous resin and adsorbs, with 8 times of column volumes, 80% ethanolic soln wash-out, collect elutriant concentrating under reduced pressure, concentrated solution is extracted with ethyl acetate, extraction liquid reclaims actual, obtains medicinal extract.Get ethyl acetate, propyl carbinol, water, 5:3:7 mixes in proportion, gets and injects mutually the chromatotube phase that fixes, engine speed 800rpm, take off and do mutually moving phase, flow velocity 3ml/min, collects flow point according to collection of illustrative plates, flow point drying under reduced pressure obtains justicidin A 1.9g, detects content 98.1% through HPLC.
Embodiment 3:
Get 5kg justicia grass raw material pulverizing, add 7 times of amount 85% alcohol reflux 3 times, merge extracted twice liquid and reclaim ethanol, concentrated solution dilute with water adds in HPD500 macroporous resin and adsorbs, with 7 times of column volumes, 60% ethanolic soln wash-out, collect elutriant concentrating under reduced pressure, concentrated solution is extracted with ethyl acetate, extraction liquid reclaims actual, obtains medicinal extract.Get ethyl acetate, propyl carbinol, water, 3:2:5 mixes in proportion, gets and injects mutually the chromatotube phase that fixes, engine speed 850rpm, take off and do mutually moving phase, flow velocity 2ml/min, collects flow point according to collection of illustrative plates, flow point drying under reduced pressure obtains justicidin A 2.1g, detects content 98.5% through HPLC.
Embodiment 4:
Get 5kg justicia grass raw material pulverizing, add 7 times of amount 80% alcohol reflux 3 times, merge extracted twice liquid and reclaim ethanol, concentrated solution dilute with water adds in NK-II macroporous resin and adsorbs, with 10 times of column volumes, 50% ethanolic soln wash-out, collect elutriant concentrating under reduced pressure, concentrated solution is extracted with ethyl acetate, extraction liquid reclaims actual, obtains medicinal extract.Get ethyl acetate, propyl carbinol, water, 4:3:6 mixes in proportion, gets and injects mutually the chromatotube phase that fixes, engine speed 900rpm, take off and do mutually moving phase, flow velocity 2ml/min, collects flow point according to collection of illustrative plates, flow point drying under reduced pressure obtains justicidin A 2.3g, detects content 97.5% through HPLC.
Claims (3)
1. a method of extracting justicidin A from justicia grass, is characterized in that following steps:
1) by justicia grass raw material pulverizing, add 7-10 doubly to measure 80-95% alcohol reflux twice, merge extracted twice liquid and reclaim ethanol, concentrated solution adds in macroporous resin and adsorbs, with 5-10 times of column volume 50-90% ethanolic soln wash-out, collect elutriant concentrating under reduced pressure, obtain concentrated solution;
2) above-mentioned concentrated solution adds ethyl acetate extraction, extraction liquid to continue to be condensed into medicinal extract to adopt high speed adverse current chromatogram to separate, collect flow point according to collection of illustrative plates, flow point drying under reduced pressure and get final product.
2. from justicia grass, extract according to claim 1 the method for justicidin A, it is characterized in that the one of the optional AB-8 of described macroporous resin, ADS-21, HPD500 and NK-II in described step 1).
3. from justicia grass, extract according to claim 1 the method for justicidin A, it is characterized in that described step 2) high speed adverse current chromatogram separation condition is: solvent systems selects ethyl acetate, propyl carbinol, water, blending ratio 2-5:1-3:3-7, get the phase that fixes mutually, the lower moving phase of doing mutually, engine speed 700-1000rpm, flow velocity 1-3ml/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410266261.8A CN104086537A (en) | 2014-06-16 | 2014-06-16 | Method for extracting justicidin A from creeping rostellularia herb |
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| CN201410266261.8A CN104086537A (en) | 2014-06-16 | 2014-06-16 | Method for extracting justicidin A from creeping rostellularia herb |
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| CN104086537A true CN104086537A (en) | 2014-10-08 |
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| CN201410266261.8A Pending CN104086537A (en) | 2014-06-16 | 2014-06-16 | Method for extracting justicidin A from creeping rostellularia herb |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957309A (en) * | 2017-03-20 | 2017-07-18 | 山东省分析测试中心 | The preparation method of lignanoids monomer in a kind of justicia |
| CN108456200A (en) * | 2017-06-22 | 2018-08-28 | 贵州省中国科学院天然产物化学重点实验室 | A kind of preparation method of 6 '-hydroxyl of high-purity-justicidin B |
-
2014
- 2014-06-16 CN CN201410266261.8A patent/CN104086537A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957309A (en) * | 2017-03-20 | 2017-07-18 | 山东省分析测试中心 | The preparation method of lignanoids monomer in a kind of justicia |
| CN106957309B (en) * | 2017-03-20 | 2019-07-30 | 山东省分析测试中心 | The preparation method of lignanoids monomer in a kind of justicia |
| CN108456200A (en) * | 2017-06-22 | 2018-08-28 | 贵州省中国科学院天然产物化学重点实验室 | A kind of preparation method of 6 '-hydroxyl of high-purity-justicidin B |
| CN108456200B (en) * | 2017-06-22 | 2021-11-09 | 贵州省中国科学院天然产物化学重点实验室 | Preparation method of high-purity 6' -hydroxy-acanthadine B |
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Application publication date: 20141008 |