CN102276465A - Method for purifying cynarin - Google Patents
Method for purifying cynarin Download PDFInfo
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- CN102276465A CN102276465A CN2011102641815A CN201110264181A CN102276465A CN 102276465 A CN102276465 A CN 102276465A CN 2011102641815 A CN2011102641815 A CN 2011102641815A CN 201110264181 A CN201110264181 A CN 201110264181A CN 102276465 A CN102276465 A CN 102276465A
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- arithoke
- ethyl acetate
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- crude extract
- extracting
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Abstract
The invention discloses a method for purifying cynarin. The method comprises the following steps of: a, taking and crushing steam leaves of artichoke, adding 4-10 times of water, heating to 45-65 DEG C, immersing and extracting for 1-2 h, extracting for 2-3 times, decompressing and condensing an extraction solution, extracting the concentrated solution by using ethyl acetate, and recovering an reagent from the extraction solution to obtain a crude extract; and b, after normal hexane, ethyl acetate, methanol and an aqueous solution are sufficiently mixed and layered, taking the bottom phase as a mobile phase and taking the top phase as a fixed phase, separating the crude extract by using a high-speed counter current chromatography, monitoring on line by using an ultraviolet detector, collecting target fractions, carrying out reduced temperature concentrating and crystallizing, and drying to obtain high-purity cynarin. The method disclosed by the invention has the advantages of rapid separation speed, short preparation period, less reagent use amount and the like. The purity of the obtained product can be up to above 98%.
Description
Technical field
The present invention relates to a kind of purification process of arithoke element, particularly relate to a kind of method that adopts high speed adverse current chromatogram purifying arithoke element.
Background technology
The arithoke element (Cynarin) be cinarine again, anghirol, colourless needle crystal (dilute acetic acid), 225～227 ℃ of fusing points, CAS 1884-23-7, molecular formula C
25H
24O
12, molecular weight 516.54, molecular structure
The arithoke element is slightly soluble in cold water, is soluble in the boiling water, is dissolved in alcohols, Glacial acetic acid etc., has the bile of enhancing and reduces fat, liver detoxification, prevention fatty liver; Can effectively suppress the oxidation of LDL cholesterol, the effect of reducing cholesterol.
The choke formal name used at school
CynarascolymusL is for composite family (Comopsite) cynara scolymus belongs to per nnial herb.The involucre of bud is edible with the holder that expands when open.Discover in the cauline leaf of choke and contain a large amount of phenolic acids, wherein the arithoke cellulose content is about 0.5%, and cauline leaf mostly is waste.
From choke, extract the method for arithoke element, general macroporous resin and the membrane separation process that adopts, the product that obtains mostly is crude extract.As patent (application number 200910107323) " method of purification of arithoke element in a kind of choke ", the method for this patent disclosure is that leaf of Cynara scolymus L passes through ethanol or acetone soln extracts, and extracting solution concentrates the back depositing in water and filters, and filtrate is carried out micro-filtration again and handles; Regulate gained dialyzate pH value, get the thick product purity of silibin by the macroporous adsorption resin chromatography post and reach more than 20%.The method for preparing high-content arithoke element, general silica gel column chromatography or preparation liquid phase separation.The loss of silicagel column sample separation is serious, and solvent load is big, and the cycle is long, and preparation liquid phase separation preparation amount is less.
Summary of the invention
The objective of the invention is to overcome the deficiency and the technological deficiency of existing method, a kind of purification process of arithoke element is provided.
The objective of the invention is to be achieved through the following technical solutions: a kind of purification process of arithoke element is characterized in that following steps:
A. get the choke cauline leaf and pulverize, add 4-10 times of water gaging, be heated to 45-65 ℃, soak and extracted 1-2 hour, extract 2-3 time, the extracting solution concentrating under reduced pressure, the concentrated solution ethyl acetate extraction, extraction liquid reclaims reagent, gets crude extract;
B. after getting normal hexane, ethyl acetate, methyl alcohol, the abundant layering of aqueous solution, take off and do moving phase mutually, on the phase that fixes mutually, adopt high speed adverse current chromatogram to separate above-mentioned crude extract, the UV-detector on-line monitoring is collected the target flow point, the concentrating under reduced pressure crystallization, the dry high purity arithoke element that gets.
Normal hexane among the described step b, ethyl acetate, methyl alcohol, aqueous solution ratio are: 1-3:5-9:2-4:6-11.
High speed adverse current chromatogram separation host rotating speed 600-1000rpm among the described step b, flow rate of mobile phase 1-4ml/min.
Advantage of the present invention is: method adopts high adverse current chromatogram method purifying arithoke element, is a kind of liquid-liquid partition chromatography, need not solid carrier, and sample separation is not had absorption, and velocity of separation is fast, and preparation amount is big, and solvent load is little and can recycle.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
The choke cauline leaf is pulverized, and gets 2kg, adds 10 times of water gagings and is heated to 65 ℃, soaks 1 hour, extracts liquid, adds 4 times of water gagings again, extract 1 time, and united extraction liquid concentrating under reduced pressure, concentrated solution adds the equal-volume ethyl acetate extraction 2 times, and extraction liquid reclaims reagent, gets medicinal extract.Get normal hexane, ethyl acetate, methyl alcohol, the aqueous solution by the 1:5:2:6 mixed, fully after the layering, get and inject the high speed adverse current chromatogram post phase that fixes mutually, rotate main frame 700rpm, pump into down and do moving phase mutually, after the running balance, flow rate of mobile phase is adjusted into 2ml/min, and dissolves medicinal extract with moving phase, by the sampling valve sample introduction, the UV-detector on-line monitoring, collect the target flow point, concentrating under reduced pressure, crystallization, the dry plain 900mg of arithoke, the content 98.5% of getting.
Embodiment 2:
The choke cauline leaf is pulverized, and gets 2kg, adds 8 times of water gagings and is heated to 45 ℃, soaks 2 hours, extracts liquid, adds 5 times of water gagings again, extract 1 time, and united extraction liquid concentrating under reduced pressure, concentrated solution adds the equal-volume ethyl acetate extraction 2 times, and extraction liquid reclaims reagent, gets medicinal extract.Get normal hexane, ethyl acetate, methyl alcohol, the aqueous solution by the 3:9:4:11 mixed, fully after the layering, get and inject the high speed adverse current chromatogram post phase that fixes mutually, rotate main frame 800rpm, pump into down and do moving phase mutually, after the running balance, flow rate of mobile phase is adjusted into 3ml/min, and dissolves medicinal extract with moving phase, by the sampling valve sample introduction, the UV-detector on-line monitoring, collect the target flow point, concentrating under reduced pressure, crystallization, the dry plain 940mg of arithoke, the content 98.1% of getting.
Claims (3)
1. the purification process of an arithoke element is characterized in that following steps:
A. get the choke cauline leaf and pulverize, add 4-10 times of water gaging, be heated to 45-65 ℃, soak and extracted 1-2 hour, extract 2-3 time, the extracting solution concentrating under reduced pressure, the concentrated solution ethyl acetate extraction, extraction liquid reclaims reagent, gets crude extract;
B. after getting normal hexane, ethyl acetate, methyl alcohol, the abundant layering of aqueous solution, take off and do moving phase mutually, on the phase that fixes mutually, adopt high speed adverse current chromatogram to separate above-mentioned crude extract, the UV-detector on-line monitoring is collected the target flow point, the concentrating under reduced pressure crystallization, the dry high purity arithoke element that gets.
2. the purification process of arithoke element as claimed in claim 1 is characterized in that normal hexane, ethyl acetate, methyl alcohol, the aqueous solution ratio among the described step b is: 1-3:5-9:2-4:6-11.
3. the purification process of arithoke element as claimed in claim 1 is characterized in that the high speed adverse current chromatogram separation host rotating speed 600-1000rpm among the described step b, flow rate of mobile phase 1-4ml/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102641815A CN102276465A (en) | 2011-09-08 | 2011-09-08 | Method for purifying cynarin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102641815A CN102276465A (en) | 2011-09-08 | 2011-09-08 | Method for purifying cynarin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102276465A true CN102276465A (en) | 2011-12-14 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102641815A Pending CN102276465A (en) | 2011-09-08 | 2011-09-08 | Method for purifying cynarin |
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| CN (1) | CN102276465A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496033A (en) * | 2016-10-17 | 2017-03-15 | 汇美农业科技有限公司 | The extracting method of 1,5 dicaffeoylquinic acids in a kind of globe artichoke |
| CN106577981A (en) * | 2016-12-16 | 2017-04-26 | 湖南文理学院 | Preparation method of globe artichoke aquatic product preservation film coating solution |
| CN108484402A (en) * | 2018-06-13 | 2018-09-04 | 爱可道生物科技有限公司 | The purifying technique of cynarin in a kind of globe artichoke |
-
2011
- 2011-09-08 CN CN2011102641815A patent/CN102276465A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496033A (en) * | 2016-10-17 | 2017-03-15 | 汇美农业科技有限公司 | The extracting method of 1,5 dicaffeoylquinic acids in a kind of globe artichoke |
| CN106577981A (en) * | 2016-12-16 | 2017-04-26 | 湖南文理学院 | Preparation method of globe artichoke aquatic product preservation film coating solution |
| CN108484402A (en) * | 2018-06-13 | 2018-09-04 | 爱可道生物科技有限公司 | The purifying technique of cynarin in a kind of globe artichoke |
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| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111214 |