CN104672187A - Preparation method of arctigenin in arctium fruit - Google Patents
Preparation method of arctigenin in arctium fruit Download PDFInfo
- Publication number
- CN104672187A CN104672187A CN201310618343.XA CN201310618343A CN104672187A CN 104672187 A CN104672187 A CN 104672187A CN 201310618343 A CN201310618343 A CN 201310618343A CN 104672187 A CN104672187 A CN 104672187A
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- CN
- China
- Prior art keywords
- arctigenin
- dichloromethane
- ethyl acetate
- silica gel
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/26—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D307/30—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/32—Oxygen atoms
- C07D307/33—Oxygen atoms in position 2, the oxygen atom being in its keto or unsubstituted enol form
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a refinement method of arctigenin in arctium fruit. The method is characterized by comprising the following steps: hydrolyzing arctiin into arctigenin by an enzymolysis process, and carrying out silica gel column chromatography to separate the arctigenin from the hydrolyzate by using dichloromethane-ethyl acetate as a mobile phase. The method has the advantages of simple technique and stable product quality.
Description
Technical field
The present invention relates to the preparation field of natural product, particularly the preparation method of l-arctigenin in a kind of Great Burdock Achene.
Background technology
L-arctigenin, another name: aretigenin, English name arctigenin.Great Burdock Achene is conventional Chinese medicine, is the dry mature fruit of composite family biennial herb plant burdock (formal name used at school: Arctium lappa L.).Life is used or is fried use, and the used time smashs to pieces.There are dispelling wind and heat pathogens, a surname's lung promoting eruption, relieve sore throat dissipating bind, effect of detoxify and promote the subsdence of swelling.Belong to wind-heat-dispersing medicinal in diaphoretic medicine.Modern study, Great Burdock Achene also can be used for preventing and treating diabetic nephropathy; The arctigenin that Arctium lappa fruit generates through hydrolysis containing arctigenin has antitumour activity.Arctinin meta structure is as follows:
Summary of the invention
The technical scheme that the present invention adopts for achieving the above object is as follows: adopt enzymolysis process that arctinin is hydrolyzed to l-arctigenin, use silica gel column chromatography, be moving phase with dichloromethane-ethyl acetate, be separated from hydrolyzate and obtain l-arctigenin, comprise following steps:
(1), by arctinin mix with synaptase, be dissolved in water, 37 DEG C prevent 48h from carrying out enzymolysis.
(2), by enzymolysis product use dichloromethane extraction, filter.
(3), by after dichloromethane extract recycling design, using silica gel column chromatography, take dichloromethane-ethyl acetate as moving phase.
(4), by the 4-5 column volume of dichloromethane-ethyl acetate elutriant concentrate, crystallization.
The present invention has following technique effect: the present invention adopts enzyme hydrolysis method to be combined with chromatography, and be separated from hydrolyzate and obtain l-arctigenin, technique is simple, constant product quality, solvent adopts ethanol, methylene dichloride, ethyl acetate, and recoverable, production cost is lower.
Embodiment:
Embodiment 1
Get arctinin 100mg to mix with synaptase 5mg, be dissolved in water, 37 DEG C prevent 48h from carrying out enzymolysis.Used by enzymolysis product methylene dichloride 50ml to extract, filter.After dichloromethane extract recycling design, use silica gel column chromatography, with dichloromethane-ethyl acetate (5:4) for moving phase, wash-out 6 column volumes are about 200ml.The 4-5 column volume of dichloromethane-ethyl acetate elutriant is concentrated, crystallization.Can obtain l-arctigenin, purity is 95.6%.
Embodiment 2
Get arctinin 500mg to mix with synaptase 25mg, be dissolved in water, 37 DEG C prevent 48h from carrying out enzymolysis.Used by enzymolysis product methylene dichloride 250ml to extract, filter.After dichloromethane extract recycling design, use silica gel column chromatography, with dichloromethane-ethyl acetate (5:4) for moving phase, wash-out 6 column volumes are about 1000ml.The 4-5 column volume of dichloromethane-ethyl acetate elutriant is concentrated, crystallization.Can obtain l-arctigenin, purity is 94.8%.
Embodiment 3
Get arctinin 1g to mix with synaptase 50mg, be dissolved in water, 37 DEG C prevent 48h from carrying out enzymolysis.Used by enzymolysis product methylene dichloride 500ml to extract, filter.After dichloromethane extract recycling design, use silica gel column chromatography, with dichloromethane-ethyl acetate (5:4) for moving phase, wash-out 6 column volumes are about 2000ml.The 4-5 column volume of dichloromethane-ethyl acetate elutriant is concentrated, crystallization.Can obtain l-arctigenin, purity is 95.4%.
Claims (1)
1. the process for purification of l-arctigenin in Great Burdock Achene, concrete steps are:
(1), by arctinin mix with synaptase, be dissolved in water, 37 DEG C prevent 48h from carrying out enzymolysis;
(2), by enzymolysis product use dichloromethane extraction, filter;
(3), by after dichloromethane extract recycling design, using silica gel column chromatography, take dichloromethane-ethyl acetate as moving phase;
(4), by the 4-5 column volume of dichloromethane-ethyl acetate elutriant concentrate, crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310618343.XA CN104672187A (en) | 2013-11-29 | 2013-11-29 | Preparation method of arctigenin in arctium fruit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310618343.XA CN104672187A (en) | 2013-11-29 | 2013-11-29 | Preparation method of arctigenin in arctium fruit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104672187A true CN104672187A (en) | 2015-06-03 |
Family
ID=53307829
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310618343.XA Pending CN104672187A (en) | 2013-11-29 | 2013-11-29 | Preparation method of arctigenin in arctium fruit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104672187A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440459A (en) * | 2018-04-03 | 2018-08-24 | 徐州工程学院 | A kind of method of high efficiency extraction arctigenin |
-
2013
- 2013-11-29 CN CN201310618343.XA patent/CN104672187A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440459A (en) * | 2018-04-03 | 2018-08-24 | 徐州工程学院 | A kind of method of high efficiency extraction arctigenin |
| CN108440459B (en) * | 2018-04-03 | 2021-03-02 | 徐州工程学院 | Method for extracting arctigenin |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150603 |