CN1398872A - Puerarin preparing process - Google Patents
Puerarin preparing process Download PDFInfo
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- CN1398872A CN1398872A CN 02133692 CN02133692A CN1398872A CN 1398872 A CN1398872 A CN 1398872A CN 02133692 CN02133692 CN 02133692 CN 02133692 A CN02133692 A CN 02133692A CN 1398872 A CN1398872 A CN 1398872A
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- puerarin
- column chromatography
- silica gel
- adsorbent resin
- macroporous adsorbent
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Abstract
The present invention is a Puerarin preparing process from Pueraria spp. plant. Water extractive of Pueraria spp. plant root is produced into high-purity Puerarin through chromatographic separation with macroporous adsorption resin, elution with ethanol solution collecting, enrichment positions, concentration, then chromatographic purification with silica gel column, organic solvent elution, and concentration. The said process uses no toxic organic solvent, reuses all the solvent, and has no "three waste" pollution and high Puerarin content in the product. The process is simple, practical, low in cost and short in production period, and is easy to use in industrial production.
Description
Technical field: the invention belongs to a kind of method of extracting puerarin from plant root.Particularly, relate to a kind of method of extracting puerarin (Puerarin) from the root of pulse family Pueraria lobota platymiscium.
Technical background: puerarin is a kind of isoflavones glycoside (C
20H
21O
9), be one of main effective constituent of the Chinese medicine root of kudzu vine.Puerarin is general preparation method have: water extraction and alcohol precipitation method, propyl carbinol one aqueous extraction method, aluminum oxide decoloring method, polymeric amide chromatography method, Glacial acetic acid crystallization process etc.The aforesaid method link is many, uses inflammable, the deleterious machine solvent of using in a large number, easily causes environmental pollution and to the infringement of operator's health, the production cost height, and the cycle is long, and impurity is many in the product, and puerarin content is low etc.
Summary of the invention: at the above-mentioned shortcoming that prior art exists, the present invention aims to provide a kind of simple, low-cost, pollution-free, the puerarin novel preparation method that have no side effect, active constituent content is high.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
A kind of method for preparing puerarin (Puerarin), Pueraria lobota is belonged to the assorted clearly drying and crushing of (Pueraria spp.) plant roots raw material, then through water extraction, concentrate, drying, water extract-macroporous adsorbent resin column chromatography separations, aqueous ethanol wash-out, concentrate, purification by silica gel column chromatography, single organic solvent wash-out, concentrate, puerarin crude product or substep collection, concentrated puerarin elaboration.
The aforesaid method raw material is chosen the root of pulse family Pueraria lobota platymiscium and other congeners.
The employed sorbent material of aforesaid method column chromatography is polystyrene type macroporous adsorbent resin and silica gel.
Aforesaid method macroporous adsorbent resin column chromatography elutriant is an aqueous ethanol, and the silica gel column chromatography elutriant is a single organic solvent as chloroform, formic acid second fat, ethyl acetate etc.
Aforesaid method is a chromatographic material with the polystyrene type macroporous adsorbent resin, and the ratio of water extract and macroporous adsorbent resin is 1: 10, and the purification by silica gel column chromatography condition is that the ratio of sample and 200-300 purpose silica gel is 1: 15.
The drying means of puerarin is except that general drying means in the aforesaid method, available lyophilize, spraying drying and microwave drying etc.
The present invention's method more specifically is that meal is mixed, cleans, dries, is ground into to Pueraria lobota platymiscium root starting material clearly, then the heating of Pueraria lobota platymiscium root meal water is extracted 2 times, each extraction time is 2 hours, then after filtration, concentrate, drying obtains water extract; Again through macroporous adsorbent resin column chromatography, water extract separates with macroporous adsorbent resin column chromatography after with 10% dissolve with ethanol, and be eluted to the elutriant colorless and odorless with 10% ethanolic soln, strengthen ethanol then, detect in conjunction with TCL, collecting wavelength is the elutriant that 254nm shows the fluorescence part, with collected elutriant thin up, diluent is used ethanol elution again through macroporous adsorbent resin column chromatography, collects elutriant and concentrated; After silica gel column chromatography with 200-300 order silica gel dress post, is a sample on 1: 15 in sample and silica gel ratio, silica gel for single organic solvent as wash-outs such as chloroform, formic acid second fat or ethyl acetates, detect in conjunction with TCL, collect elutriant, concentrate drying promptly obtains highly purified puerarin.
Compared with prior art, method of the present invention has following advantage:
1, the present invention extracts puerarin from the root of pulse family Pueraria lobota platymiscium (as: elegant jessamine Pueraria lobata (Will.) Ohwi, Pachyrhizua angulatus (P.thomsonii Benth.) and other congeners).And in method, with the means of thin-layer chromatography (TCL) as each link of monitoring technical process.Products obtained therefrom yield height, good product performance has no side effect, the active constituent content height.
2, the used material of column chromatography is respectively polystyrene type macroporous adsorbent resin and silica gel in the inventive method, elutriant is respectively aqueous ethanol and single organic solvent (as: chloroform, formic acid second fat, ethyl acetate etc.), wherein macroporous adsorbent resin can be reused, ethanol and organic solvent all can be recycled, reduce production cost widely, reduced environmental pollution.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is puerarin standard substance HPLC of the present invention;
Fig. 3 is root of kudzu vine water extract HPLC of the present invention, and puerarin content is 29.40%;
Fig. 4 is the HPLC of water extract of the present invention after macroporous adsorbent resin separates, and puerarin content is 47.06%;
Fig. 5 is the puerarin HPLC behind the purification by silica gel column chromatography of the present invention, and puerarin content is 77.5%;
Fig. 6 is that purification by silica gel column chromatography of the present invention, substep are collected puerarin elaboration HPLC, and puerarin content is 93.59%;
Fig. 7 is the structural representation of puerarin of the present invention.
Embodiment:
Further specify essentiality content of the present invention below in conjunction with embodiments of the invention, but content of the present invention is not limited thereto.
Embodiment 1:
(1) meal is mixed, cleans, dries, is ground into to the root of getting elegant jessamine (P.lobata) clearly for 1 kilogram;
(2) root of kudzu vine meal water heating is extracted 2 times, each extraction time is 2 hours, then after filtration, concentrate, drying obtains root of kudzu vine water extract;
(3) macroporous adsorbent resin column chromatography: water extract 800 grams, after dissolve with ethanol solution with 10% filters, with macroporous adsorptive resins (post is high 130 centimetres, diameter 9 centimetres) chromatographic separation, ethanolic soln with 10% is eluted to the elutriant colorless and odorless, use the aqueous ethanol wash-out again, detect (wavelength is 254nm) in conjunction with TCL, till elutriant does not contain puerarin; To containing ethanol below 10%, diluting soln by macroporous adsorbent resin column chromatography, is used ethanol elution again with collected elutriant thin up, collects elutriant and concentrate to obtain concentrated extract 400 grams.
(4) silica gel column chromatography: in sample on sample and the silica gel ratio 1: 15, silica gel is the 200-300 order, use the single organic solvent wash-out, detect substep in conjunction with TCL and collect elutriant, concentrate drying promptly obtains highly purified puerarin, detect through HPLC, calculate with aqueous extract, average purity is 77.5%, and yield is 26%, wherein purity greater than 90% puerarin elaboration puerarin, 160 grams, yield is 16%.
Claims (7)
1. method for preparing puerarin (Puerarin), it is characterized in that Pueraria lobota is belonged to the assorted clearly drying and crushing of (Pueraria spp.) plant roots raw material, then through water extraction, concentrate, drying, water extract-macroporous adsorbent resin column chromatography separations, aqueous ethanol wash-out, concentrate, purification by silica gel column chromatography, single organic solvent wash-out, concentrate, puerarin crude product or substep collection, concentrated puerarin elaboration.
2. method according to claim 1 is characterized in that raw material chooses the root of pulse family Pueraria lobota platymiscium and other congeners.
3. method according to claim 1 is characterized in that the employed sorbent material of column chromatography is polystyrene type macroporous adsorbent resin and silica gel.
4. method according to claim 1 is characterized in that the macroporous adsorbent resin column chromatography elutriant is an aqueous ethanol, and the silica gel column chromatography elutriant is a single organic solvent as chloroform, formic acid second fat, ethyl acetate etc.
5. method according to claim 1, it is characterized in that with the polystyrene type macroporous adsorbent resin be chromatographic material, the ratio of water extract and macroporous adsorbent resin is 1: 10, and the purification by silica gel column chromatography condition is that the ratio of sample and 200-300 purpose silica gel is 1: 15.
6. method according to claim 1 is characterized in that the puerarin drying means except that general drying means, available lyophilize, spraying drying and microwave drying etc.
7. according to claim 1 or 2 or 3 or 4 or 5 or 6 described methods, it is characterized in that meal is mixed, cleans, dries, is ground into to Pueraria lobota platymiscium root starting material clearly, then the heating of Pueraria lobota platymiscium root meal water is extracted 2 times, each extraction time is 2 hours, then after filtration, concentrate, drying obtains water extract; Again through macroporous adsorbent resin column chromatography, water extract separates with macroporous adsorbent resin column chromatography after with 10% dissolve with ethanol, and be eluted to the elutriant colorless and odorless with 10% ethanolic soln, strengthen ethanol then, detect in conjunction with TCL, collecting wavelength is the elutriant that 254nm shows the fluorescence part, with collected elutriant thin up, diluent is used ethanol elution again through macroporous adsorbent resin column chromatography, collects elutriant and concentrated; After silica gel column chromatography with 200-300 order silica gel dress post, is a sample on 1: 15 in sample and silica gel ratio, silica gel for single organic solvent as wash-outs such as chloroform, formic acid second fat or ethyl acetates, detect in conjunction with TCL, collect elutriant, concentrate drying promptly obtains highly purified puerarin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02133692XA CN1169820C (en) | 2002-08-29 | 2002-08-29 | Puerarin preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02133692XA CN1169820C (en) | 2002-08-29 | 2002-08-29 | Puerarin preparing process |
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| Publication Number | Publication Date |
|---|---|
| CN1398872A true CN1398872A (en) | 2003-02-26 |
| CN1169820C CN1169820C (en) | 2004-10-06 |
Family
ID=4747339
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB02133692XA Expired - Fee Related CN1169820C (en) | 2002-08-29 | 2002-08-29 | Puerarin preparing process |
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| CN (1) | CN1169820C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318955B (en) * | 2007-06-08 | 2010-12-22 | 中国科学院大连化学物理研究所 | Method for preparing effective component of kudzu root |
| CN101941966A (en) * | 2010-09-07 | 2011-01-12 | 南通诚信氨基酸有限公司 | Method for extracting high-purity puerarin |
| CN1927876B (en) * | 2005-09-07 | 2011-01-19 | 天津天士力现代中药资源有限公司 | Method for extracting and preparing puerarin |
| CN102532111A (en) * | 2010-12-24 | 2012-07-04 | 天津中新药业集团股份有限公司第六中药厂 | Method for extracting puerarin from traditional Chinese medicine kudzu |
| CN102936242A (en) * | 2012-11-28 | 2013-02-20 | 云南省农业科学院药用植物研究所 | Method for comprehensively utilizing arrowroot |
| CN103224491A (en) * | 2013-05-22 | 2013-07-31 | 天津道谷生物科技有限公司 | Method for extracting high-purity puerarin by using water as solvent |
| CN108743654A (en) * | 2018-08-03 | 2018-11-06 | 哈尔滨医科大学 | It is a kind of to be used to treat Chinese medicine composition of ischemic heart disease and its preparation method and application |
| CN108947988A (en) * | 2018-08-13 | 2018-12-07 | 安徽兆龙生物科技有限公司 | A method of extracting high purity puerarin from pueraria lobata |
-
2002
- 2002-08-29 CN CNB02133692XA patent/CN1169820C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1927876B (en) * | 2005-09-07 | 2011-01-19 | 天津天士力现代中药资源有限公司 | Method for extracting and preparing puerarin |
| CN101318955B (en) * | 2007-06-08 | 2010-12-22 | 中国科学院大连化学物理研究所 | Method for preparing effective component of kudzu root |
| CN101941966A (en) * | 2010-09-07 | 2011-01-12 | 南通诚信氨基酸有限公司 | Method for extracting high-purity puerarin |
| CN102532111A (en) * | 2010-12-24 | 2012-07-04 | 天津中新药业集团股份有限公司第六中药厂 | Method for extracting puerarin from traditional Chinese medicine kudzu |
| CN102532111B (en) * | 2010-12-24 | 2016-04-27 | 天津中新药业集团股份有限公司第六中药厂 | A kind of method extracting puerarin from Chinese medicine elegant jessamine |
| CN102936242A (en) * | 2012-11-28 | 2013-02-20 | 云南省农业科学院药用植物研究所 | Method for comprehensively utilizing arrowroot |
| CN103224491A (en) * | 2013-05-22 | 2013-07-31 | 天津道谷生物科技有限公司 | Method for extracting high-purity puerarin by using water as solvent |
| CN108743654A (en) * | 2018-08-03 | 2018-11-06 | 哈尔滨医科大学 | It is a kind of to be used to treat Chinese medicine composition of ischemic heart disease and its preparation method and application |
| CN108743654B (en) * | 2018-08-03 | 2021-04-27 | 哈尔滨医科大学 | Traditional Chinese medicine composition for treating ischemic heart disease and preparation method and application thereof |
| CN108947988A (en) * | 2018-08-13 | 2018-12-07 | 安徽兆龙生物科技有限公司 | A method of extracting high purity puerarin from pueraria lobata |
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| Publication number | Publication date |
|---|---|
| CN1169820C (en) | 2004-10-06 |
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Granted publication date: 20041006 Termination date: 20110829 |