CN100443493C - Process of preparing burdock glucoside and glucosidgen thereof - Google Patents
Process of preparing burdock glucoside and glucosidgen thereof Download PDFInfo
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- CN100443493C CN100443493C CNB2006100467974A CN200610046797A CN100443493C CN 100443493 C CN100443493 C CN 100443493C CN B2006100467974 A CNB2006100467974 A CN B2006100467974A CN 200610046797 A CN200610046797 A CN 200610046797A CN 100443493 C CN100443493 C CN 100443493C
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- aglycon
- arctinin
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- aqueous alcohol
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Abstract
The present invention provides a process of preparing burdock glucoside and the glucosidgen thereof, which is a process of separating and purifying burdock glucoside and the glucosidgen thereof from burdock extract liquid through a polyamide column. The glucoside and the glucosidgen thereof prepared by the present invention can be singly or combined with other medicines as a crude drug and can be applied to medicine preparations for treating various relevant diseases. The process has the progress and practicability that the glucoside and the glucosidgen thereof prepared by the present invention have the advantages of high purity and simple, convenient and practical method and are suitable for industrial production.
Description
(1) technical field
The present invention relates to a kind of extract drugs preparation method, be specifically related to the preparation method of arctinin and aglycon thereof.Method of the present invention is meant the method by polyamide column separation and purification arctinin and aglycon thereof from Fructus Arctii extract liquid.
(2) background technology
Great Burdock Achene is the fruit of feverfew burdock (Arctium lappa L), in China various places distribution is arranged all.Great Burdock Achene records that " Chinese pharmacopoeia has dispelling wind and heat pathogens, a surname's lung promoting eruption, the effect of resolving toxin and disinhibiting the throat in going through version.Be used for the treatment of common cold due to wind-heat clinically, coughing with a lot of sputum, measles, rubella, swelling and pain in the throat, the mumps erysipelas, carbuncle sore tumefacting virus etc. are traditional Chinese medical science relieving superficies by cooling medicines commonly used.Our result of study show arctinin and aglycon thereof be the Great Burdock Achene relieving superficies by cooling effective constituent (the external anti-influenza virus activity of aretigenin. herbal medicine 2002,33 (8): 724-726; Studies on the Calcium Antagonist Action of Arctigenin.Chinese Traditional and Herbal Drugs 2000,31 (10): 758-762).Therefore Arctiin and aglycon thereof can be used as the medicament that the bulk drug preparation has antiviral, antibiotic and step-down etc.
The preparation method of present arctinin (can be called for short Arctiin) and aglycon thereof, main alcohol extracting, degreasing, the ethyl acetate extraction way (Chinese patent: have the preparation method of the Fructus Arctii extract of anti diabetes and kidney disease effect, publication number: CN1491674A) of binding silica gel column chromatography simultaneously that adopts.The solvent extration cost is higher, demixing of solvents control difficulty.
(3) summary of the invention
The objective of the invention is to use the method that simple and practical method prepares higher Arctiin of purity and aglycon thereof.
The object of the present invention is achieved like this:
A kind of method for preparing arctinin and aglycon thereof, it is characterized in that getting the Great Burdock Achene medicinal material, be ground into meal, behind the organic solvent degreasing, use the aqueous alcohol refluxing extraction, extracting liquid filtering, merging filtrate, being evaporated to medicinal extract does not have the alcohol flavor, separate through polyamide column chromatography, water, aqueous alcohol wash-out successively, with the aqueous alcohol concentrating under reduced pressure, the extract of dry arctinin and aglycon thereof.This extract can be used as bulk drug and is applied in the preparation of various treating correlative diseases.
The degreasing of Great Burdock Achene meal can be adopted low polar organic solvent such as sherwood oil, ether, chloroform and benzene, wherein adopt sherwood oil to be advisable, consumption be the Great Burdock Achene powder 8-16 doubly, can adopt modes such as ultrasonic, cold soaking and reflux, wherein the mode of reflux is good.
In the refluxing extraction operation of aqueous alcohol, the concentration of aqueous alcohol is 50-95%, and consumption is that 8-12 doubly measures, refluxing extraction 2-3 time, and each 2-3 hour, alcohol can be selected methyl alcohol or ethanol for use, is excellent with ethanol.
Alcohol extract filters, and being evaporated to does not have the alcohol flavor, and the gained fluid extract separates through the polyamide column of 0.5-2 times of Great Burdock Achene meal amount, and wherein the consumption of polymeric amide is advisable with 0.5-1 Great Burdock Achene meal amount doubly.
Polyamide column is water, 30-70% aqueous alcohol wash-out respectively, and 30-70% aqueous alcohol eluate is through concentrating under reduced pressure, the extract of dry arctinin and aglycon thereof.Alcohol can be selected methyl alcohol or ethanol for use.Adopt pure concentration difference will directly influence the yield and the content of final Arctiin and aglycon thereof.The exsiccant unit operation can adopt 50 ℃ of following vacuum-dryings or spraying drying.
The yield of prepared arctinin of present method and aglycon extract thereof is 5-15%, and the content of arctinin and aglycon thereof is 40-95% (employing high effective liquid chromatography for measuring).
This extract can be applied in the medicament of various treating correlative diseases as bulk drug separately or with the other medicines combination.
What the present invention was different with existing document or patent is: adopt polyamide column chromatography to separate Arctiin and aglycon thereof in the Great Burdock Achene, avoided operational difficulty, solvent method and silica gel column chromatography that cost is high.Use prepared arctinin of present method and aglycon purity height thereof and have advance and practical value.Simple and practical, the strong operability of present method is fit to suitability for industrialized production.
(4) embodiment
Describe the present invention for example with implementation column below, but these embodiment must not be interpreted as the restriction to claim of the present invention of going up in all senses.
Embodiment one
The Great Burdock Achene pulverizing medicinal materials becomes meal, and with 10 times of amount sherwood oil reflux degreasing 2 times, residue is waved the sherwood oil that disperses, and measures 70% alcohol reflux 2 times with 10 times then, and each 2 hours, filter, merging filtrate, being evaporated to does not have the alcohol flavor.The gained fluid extract separates with the polymeric amide of 1 times of medicinal material amount, washes with water earlier, uses the 30-70% ethanol elution again, the alcohol eluen concentrating under reduced pressure, and vacuum-drying gets the extract of arctinin and aglycon thereof, and yield is 5-15%, and the two content reaches 40-95%.
Embodiment two
Use the preparation method of Arctiin of the present invention and aglycon thereof, prepare extract.The content assaying method of Arctiin and aglycon thereof is as follows:
The content assaying method of Arctiin is according to " method under 2005 editions burdock subitems of Chinese pharmacopoeia is measured, and condition determination is: anti-phase ODS post; Moving phase is: MeOH-H
2O (1: 1.1); UV280 detects.Theoretical plate number is calculated by the Arctiin peak should be not less than 1500.The reference substance of Arctiin and aglycon thereof is this laboratory self-control.The employing external standard method is quantitative, and the two content is 40-95%.
Claims (10)
1, a kind of method for preparing arctinin and aglycon thereof, it is characterized in that getting the Great Burdock Achene medicinal material, be ground into meal, after low polar organic solvent degreasing, use the aqueous alcohol refluxing extraction, extracting liquid filtering, merging filtrate, being evaporated to medicinal extract does not have the alcohol flavor, separate through polyamide column chromatography, water, aqueous alcohol wash-out successively, with the aqueous alcohol concentrating under reduced pressure, the extract of dry arctinin and aglycon thereof.
2, a kind of method for preparing arctinin and aglycon thereof according to claim 1 is characterized in that the low polar organic solvent of degreasing employing of Great Burdock Achene meal is sherwood oil, ether, chloroform and benzene.
3, a kind of method for preparing arctinin and aglycon thereof according to claim 1 is characterized in that wherein adopting sherwood oil, and consumption is 8-16 a times of Great Burdock Achene powder.
4, a kind of method for preparing arctinin and aglycon thereof according to claim 1 is characterized in that described aqueous alcohol refluxing extraction, and the concentration of aqueous alcohol is 50-95%, and consumption is that 8-12 doubly measures, refluxing extraction 2-3 time, each 2-3 hour.
5, a kind of method for preparing arctinin and aglycon thereof according to claim 1 is characterized in that alcohol extract filters, and being evaporated to does not have the alcohol flavor, and the gained fluid extract separates through the polyamide column of 0.5-2 times of Great Burdock Achene meal amount.
6, a kind of method for preparing arctinin and aglycon thereof according to claim 1 is characterized in that wherein the consumption of polymeric amide is a 0.5-1 Great Burdock Achene meal amount doubly.
7, a kind of method for preparing arctinin and aglycon thereof according to claim 1 is characterized in that polyamide column respectively water, 30-70% aqueous alcohol wash-out, and 30-70% aqueous alcohol eluate is through concentrating under reduced pressure, the extract of dry arctinin and aglycon thereof.
8, a kind of method for preparing arctinin and aglycon thereof according to claim 7, it is characterized in that aqueous alcohol concentrates after, dry 50 ℃ of following vacuum-dryings or the spraying drying of adopting.
9, a kind of method for preparing arctinin and aglycon thereof according to claim 1, the yield that it is characterized in that gained arctinin and aglycon extract thereof is 5-15%.
10, a kind of method for preparing arctinin and aglycon thereof according to claim 1 is characterized in that the content of arctinin in gained arctinin and the aglycon extract thereof and aglycon thereof is 40-95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100467974A CN100443493C (en) | 2006-06-02 | 2006-06-02 | Process of preparing burdock glucoside and glucosidgen thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100467974A CN100443493C (en) | 2006-06-02 | 2006-06-02 | Process of preparing burdock glucoside and glucosidgen thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1861621A CN1861621A (en) | 2006-11-15 |
| CN100443493C true CN100443493C (en) | 2008-12-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100467974A Expired - Fee Related CN100443493C (en) | 2006-06-02 | 2006-06-02 | Process of preparing burdock glucoside and glucosidgen thereof |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2412377B1 (en) * | 2009-03-27 | 2018-12-26 | Kracie Holdings Ltd. | Burdock fruit extract containing arctigenin at high content and process for producing same |
| CN101736050B (en) * | 2009-12-08 | 2012-07-18 | 辽宁中医药大学 | Preparation method of arctigenin |
| CN101863937B (en) * | 2010-06-11 | 2012-07-04 | 浙江大学 | Method for preparing arctiin |
| CN102351926B (en) * | 2011-10-09 | 2015-08-05 | 苏州大学 | A kind of preparation method of arctinin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1560265A (en) * | 2004-02-26 | 2005-01-05 | 广州中医药大学 | Preparation process of burduck protoglucoside of anti virus and antiptmour natural medicine |
| CN1569019A (en) * | 2004-05-12 | 2005-01-26 | 四川发展中药现代化基地药物研究所 | Application of arctium fruit glycoside in the preparing process of nephritis treating medicine |
| CN1569138A (en) * | 2004-05-13 | 2005-01-26 | 上海交通大学 | Preparation method of arctium fruit extract for decreasing blood sugar |
-
2006
- 2006-06-02 CN CNB2006100467974A patent/CN100443493C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1560265A (en) * | 2004-02-26 | 2005-01-05 | 广州中医药大学 | Preparation process of burduck protoglucoside of anti virus and antiptmour natural medicine |
| CN1569019A (en) * | 2004-05-12 | 2005-01-26 | 四川发展中药现代化基地药物研究所 | Application of arctium fruit glycoside in the preparing process of nephritis treating medicine |
| CN1569138A (en) * | 2004-05-13 | 2005-01-26 | 上海交通大学 | Preparation method of arctium fruit extract for decreasing blood sugar |
Non-Patent Citations (2)
| Title |
|---|
| 牛蒡苷的制备与纯化. 王劲，侯凤飞，康廷国，杨松松，李程，林雅静.中草药，第33卷第9期. 2002 |
| 牛蒡苷的制备与纯化. 王劲，侯凤飞，康廷国，杨松松，李程，林雅静.中草药，第33卷第9期. 2002 * |
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| CN1861621A (en) | 2006-11-15 |
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