CN106749309A - A kind of method of the extraction purification maackiain from subprostrate sophora - Google Patents
A kind of method of the extraction purification maackiain from subprostrate sophora Download PDFInfo
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- CN106749309A CN106749309A CN201611268257.0A CN201611268257A CN106749309A CN 106749309 A CN106749309 A CN 106749309A CN 201611268257 A CN201611268257 A CN 201611268257A CN 106749309 A CN106749309 A CN 106749309A
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- Prior art keywords
- maackiain
- subprostrate sophora
- extraction purification
- ethanol
- extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/14—Ortho-condensed systems
Abstract
The invention discloses a kind of method of the extraction purification maackiain from subprostrate sophora, comprise the following steps：Extract：By subprostrate sophora pulverizing medicinal materials, aqueous solutions of organic solvent ultrasonic extraction is used, extract solution filtering obtains total alkaloids of subprostrate sophora root extract after filtrate concentration through macropore macroreticular resin post separation；Separate：By alkaloid extract through polyamide column adsorbing separation, recrystallization is obtained final product.The method process is simple, the regeneration of easy to operate, material therefor are simple, small toxicity pollution is small, are adapted to industrialized production, and maackiain purity obtained by extraction purification is high.
Description
Technical field
The present invention relates to Chemistry for Chinese Traditional Medicine field, and in particular to a kind of method of the extraction purification maackiain from subprostrate sophora.
Background technology
Subprostrate sophora, alias root of subprostrate sophora is the dry root of legume sophora tonkinensis Gapnep Sophora tonkinensis Gagnep.
And rhizome, it is China's traditional Chinese medicine.The effect of with clearing heat and detoxicating, reducing pharyngeal swelling, pented up for treating fiery poison, abscess of throat,
Gingivitis, the disease such as jaundice with damp-heat pathogen and arrhythmia cordis, hepatitis, liver cancer.Contain abundant alkaloid, flavones, three in subprostrate sophora
The various active composition such as terpene.
Maackiain is a kind of flavone component in subprostrate sophora, and its molecular formula is C16H12O5, and molecular weight is 284.267.
Maackiain has very strong antifungic action, and concentration can just suppress the growth of fungi, to leukaemia to 10 μ g/ml
(HL-60) and Rat basophilic cells leukaemia (RBL-2H3) have cytotoxic activity.
Yet there are no the relevant report of the extraction purification maackiain from subprostrate sophora.
The disclosure of background above technology contents is only used for auxiliary and understands inventive concept of the invention and technical scheme, and it is not
Necessarily belong in the prior art of present patent application, the applying date of the above in present patent application is being shown without tangible proof
In the case of disclosed, above-mentioned background technology should not be taken to evaluate the novelty and creativeness of the application.
The content of the invention
It is high it is an object of the invention to provide a kind of purity, it is adaptable to which that the extraction purification from subprostrate sophora of industrialized production is high
The method of beautiful Chinese scholartree element.
The technical solution adopted in the present invention is as follows：
A kind of method of the extraction purification maackiain from subprostrate sophora, comprises the following steps：
(1) weigh subprostrate sophora medicinal material, plus organic solvent the aqueous solution, ultrasonic extraction filtering, filtrate recycling ethanol is to without alcohol
After taste, extracted 5 times with isometric ethyl acetate, combined ethyl acetate extract, it is big in resulting solution after reclaiming ethyl acetate
Hole resin column, is eluted with 30%, 70%, 95% ethanol solution successively, collects 70% ethanol eluate, reclaims ethanol, is obtained
Solution；
(2) step (1) resulting solution is taken, upper polyamide column is eluted with methyl alcohol, collects meoh eluate, after reclaiming methyl alcohol,
It is concentrated under reduced pressure into dry, obtains solid；
(3) recrystallize：The solid solvent that step (2) is obtained is recrystallized repeatedly, is obtained final product.
Pulverizing medicinal materials mistake described in the method for the above extraction purification maackiain from subprostrate sophora, wherein step (1)
40-60 mesh sieves；The aqueous solution of the organic solvent is 70% ethanol solution, and addition is measured for 10-20 times；The ultrasonic extraction
Number of times is 3-5 times, each 1h；The macroreticular resin is HPD100 macroreticular resins, and blade diameter length ratio is 1:8-10；The amount of the eluent
For 3-5 times is measured column volume, elution flow rate is 1-2ml/min.
Polyamide column described in the method for the above extraction purification maackiain from subprostrate sophora, wherein step (2)
Blade diameter length ratio is 1:10-15；The amount of the eluent measures column volume for 3-5 times, and elution flow rate is 1-2ml/min.
In the method for the extraction purification maackiain from subprostrate sophora, solvent is methyl alcohol, second wherein described in step (3)
Alcohol or acetone；Solid is 1g with the amount ratio of solvent：(1-10)ml.
Beneficial effects of the present invention：
What the 1st, the present invention was provided separates the material regeneration letter for using from subprostrate sophora in the method for extraction purification maackiain
Single, small toxicity pollution is small, is adapted to industrialized production.
2nd, the maackiain purity obtained by the inventive method extraction purification is high, more than 98.0%.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but do not limit the scope of the invention and apply
Scope：
Embodiment 1
Subprostrate sophora medicinal material 50g is weighed, 40 mesh sieves were crushed, plus 10 times of 70% ethanol solutions of amount, ultrasonic extraction 3 times, every time
1h, filtering, filtrate recycling ethanol is extracted 5 times, combined ethyl acetate extract to after without alcohol taste with isometric ethyl acetate,
After reclaiming ethyl acetate, (blade diameter length ratio is 1 to HPD100 macroporous resin columns in resulting solution:8), column volume is measured with 3 times successively
30%th, 70%, 95% ethanol solution is eluted, and elution flow rate is that 1ml/min collects 70% ethanol eluate, reclaims ethanol
Afterwards, in resulting solution polyamide column (blade diameter length ratio is 1:10), eluted with the methyl alcohol of 3 times of amount column volumes, elution flow rate is 1ml/
Min, collects meoh eluate, after reclaiming methyl alcohol, is concentrated under reduced pressure into dry, obtains the dissolving of solid methyl alcohol, the consumption of solid and solvent
Than being 1g:1ml, recrystallizes to maackiain crystallization completely repeatedly, obtains maackiain 0.27g, and content is 99.80%.
Embodiment 2
Subprostrate sophora medicinal material 100g is weighed, 50 mesh sieves were crushed, plus 15 times of 70% ethanol solutions of amount, ultrasonic extraction 4 times, every time
1h, filtering, filtrate recycling ethanol is extracted 5 times, combined ethyl acetate extract to after without alcohol taste with isometric ethyl acetate,
After reclaiming ethyl acetate, (blade diameter length ratio is 1 to HPD100 macroporous resin columns in resulting solution:9), column volume is measured with 4 times successively
30%th, 70%, 95% ethanol solution is eluted, and elution flow rate is that 1.5ml/min collects 70% ethanol eluate, reclaims ethanol
Afterwards, in resulting solution polyamide column (blade diameter length ratio is 1:12), eluted with the methyl alcohol of 4 times of amount column volumes, elution flow rate is 1.5ml/
Min, collects meoh eluate, after reclaiming methyl alcohol, is concentrated under reduced pressure into dry, is dissolved with ethanol, and the amount ratio of solid and ethanol is 1g:
5ml, is concentrated into maackiain crystallization completely, obtains maackiain 0.53g, and content is 99.82%.
Embodiment 3
Subprostrate sophora medicinal material 200g is weighed, 60 mesh sieves were crushed, plus 20 times of 70% ethanol solutions of amount, ultrasonic extraction 5 times, every time
1h, filtering, filtrate recycling ethanol is extracted 5 times, combined ethyl acetate extract to after without alcohol taste with isometric ethyl acetate,
After reclaiming ethyl acetate, (blade diameter length ratio is 1 to HPD100 macroporous resin columns in resulting solution:10), column volume is measured with 5 times successively
30%th, 70%, 95% ethanol solution is eluted, and elution flow rate is that 2ml/min collects 70% ethanol eluate, reclaims ethanol
Afterwards, in resulting solution polyamide column (blade diameter length ratio is 1:15), eluted with the methyl alcohol of 5 times of amount column volumes, elution flow rate is 2ml/
Min, collects meoh eluate, after reclaiming methyl alcohol, is concentrated under reduced pressure into dry, obtains solid acetone solution, the consumption of solid and acetone
Than being 1g:10ml, is concentrated into maackiain crystallization completely, obtains maackiain 1.05g, and content is 99.81%.
Above content is to combine specific/preferred embodiment further description made for the present invention, it is impossible to
Assert that specific implementation of the invention is confined to these explanations.Come for general technical staff of the technical field of the invention
Say, without departing from the inventive concept of the premise, its embodiment that can also have been described to these makes some replacements or modification,
And these are substituted or variant should all be considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of method of the extraction purification maackiain from subprostrate sophora, it is characterised in that comprise the following steps：
(1) weigh subprostrate sophora medicinal material, plus organic solvent the aqueous solution, ultrasonic extraction, filtering, filtrate recycling ethanol is to without alcohol taste
Afterwards, extracted 5 times with isometric ethyl acetate, combined ethyl acetate extract, after reclaiming ethyl acetate, macropore in resulting solution
Resin column, is eluted with 30%, 70%, 95% ethanol solution successively, collects 70% ethanol eluate, reclaims ethanol, obtains molten
Liquid；
(2) step (1) resulting solution is taken, upper polyamide column is eluted with methyl alcohol, collects meoh eluate, after reclaiming methyl alcohol, decompression
It is concentrated to dryness, obtains solid；
(3) recrystallize：The solid solvent that step (2) is obtained is recrystallized repeatedly, is obtained final product.
2. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(1) pulverizing medicinal materials described in cross 40-60 mesh sieves.
3. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(1) aqueous solution of organic solvent described in is 70% ethanol solution, and addition is measured for 10-20 times.
4. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(1) number of times of ultrasonic extraction described in is 3-5 times, each 1h.
5. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(1) macroreticular resin described in is HPD100 macroreticular resins.
6. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(1) blade diameter length ratio of macroporous resin column described in is 1:8-10.
7. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(1) amount of eluent described in measures column volume for 3-5 times, and elution flow rate is 1-2ml/min.
8. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(2) blade diameter length ratio of polyamide column described in is 1:10-15.
9. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(2) amount of eluent described in measures column volume for 3-5 times, and elution flow rate is 1-2ml/min.
10. a kind of method of the extraction purification maackiain from subprostrate sophora according to claim 1, it is characterised in that step
(3) solvent described in is methyl alcohol, ethanol or acetone；Solid is 1g with the amount ratio of solvent：(1-10)ml.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478567A (en) * | 2022-03-03 | 2022-05-13 | 中国科学院新疆理化技术研究所 | Method for preparing pterocarpan compounds of Korean sophoricine and Meidi pterocarpan from chickpea sprouts |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1633301A (en) * | 2000-06-29 | 2005-06-29 | 威廉施瓦布博士有限公司 | Extracts from sophora,production method and purposes thereof |
-
2016
- 2016-12-31 CN CN201611268257.0A patent/CN106749309A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1633301A (en) * | 2000-06-29 | 2005-06-29 | 威廉施瓦布博士有限公司 | Extracts from sophora,production method and purposes thereof |
Non-Patent Citations (3)
| Title |
|---|
| 施顺东等: "广豆根的化学成分研究", 《湖北农业科学》 * |
| 邓银华等: "山豆根化学成分研究", 《天然产物研究与开发》 * |
| 隆金桥等: "广西山豆根化学成分的研究", 《云南大学学报（自然科学版）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478567A (en) * | 2022-03-03 | 2022-05-13 | 中国科学院新疆理化技术研究所 | Method for preparing pterocarpan compounds of Korean sophoricine and Meidi pterocarpan from chickpea sprouts |
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