CN102911146A - Method for extracting tricin from alfalfa - Google Patents
Method for extracting tricin from alfalfa Download PDFInfo
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- CN102911146A CN102911146A CN2011102186872A CN201110218687A CN102911146A CN 102911146 A CN102911146 A CN 102911146A CN 2011102186872 A CN2011102186872 A CN 2011102186872A CN 201110218687 A CN201110218687 A CN 201110218687A CN 102911146 A CN102911146 A CN 102911146A
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Abstract
The invention belongs to the technical field of biology, and discloses a method for extracting tricin from alfalfa. The method is characterized in comprising the steps that: (1) alfalfa is crushed; 5-8 time amount of 60-80% ethanol is added for carrying out reflux extraction 2-3 times; an obtained extraction liquid is concentrated until no alcohol is left; the extraction liquid is absorbed by using polyamide resin column; an ethanol solution is used in gradient elution; thin-layer detection is carried out; high-concentration fraction is collected and concentrated; ethyl acetate is added for extracting; and ethyl acetate is recovered, such that a crude product is obtained; (2) n-hexane, ethyl acetate, methanol, and water are mixed; an upper-phase is used for filling a high-speed countercurrent chromatographic column; a main machine is rotated, and a lower-phase is pumped in as a mobile phase; the crude product dissolved by the mobile phase is fed by using a feeding valve, and is subjected to UV detector online monitoring; a target component is collected; obtained fractions are combined; and the mixture is subjected to reduced-pressure drying, such that high-purity tricin is obtained. The method provided by the invention has the advantages of short-period, simple operation, large preparation amount, high yield, and the like. The method is suitable for preparations of high-purity tricin.
Description
Technical field
The invention belongs to biological technical field, especially relate to a kind of method of from alfalfa, extracting Tricin.
Background technology
Tricin is again tricin, Wheat flavone, chemical name 5,7-dihydroxyl-2-(4-hydroxyl-3,5-Dimethoxyphenyl) benzopyran-4-one, CAS 520-32-1, fusing point 285-286 ℃, molecular formula C17H1407, molecular weight 330, molecular structural formula
Tricin is a kind of Flavonoid substances, has slight antioxygenation, and anti-smooth muscle loosening and antitumor action also have the dyeing function.
Tricin extensively exists in the plant, but content is lower, is not enough to separation and purification, and content is more in alfalfa.Mostly the method for preparing the high purity Tricin is to adopt solid-filling post method, such as silicagel column, reverse phase silica gel post and gel column method.This separation method sample loss is serious, complex operation, poor reproducibility.Such as patent (application number 201010605530) " method that from the leaf of bamboo, prepares the high purity Tricin ", the method for this patent disclosure: the dry leaf of bamboo 95% extraction using alcohol, use petroleum ether extraction, water is condensed into medicinal extract; Make AB-8 macroporous resin column on the medicinal extract, use first the pure water wash-out, use again 80% ethanol elution, elutriant is concentrated and dry; Add methanol hydrochloride solution in the desciccate, heating is carried out acidolysis and is processed; C18 column chromatography wash-out on the gained acid hydrolysis solution is collected the Tricin fraction, and is concentrated; Gel separator column on the gained enriched material is made the moving phase wash-out with pure methyl alcohol, collects the Tricin fraction, is concentrated to drying, namely gets Tricin.
Summary of the invention
The objective of the invention is to overcome now methodical defective, a kind of method of extracting Tricin from alfalfa is provided.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of extracting Tricin from alfalfa is characterized in that following steps:
1) alfalfa is pulverized, and adds 5-8 and doubly measures the 60-80% alcohol reflux 2-3 time, and extracting solution is concentrated into without alcohol, add in the polyamide resin and adsorb, the ethanolic soln gradient elution, thin layer detects, add ethyl acetate extraction after collection high density flow point is concentrated, reclaim ethyl acetate and get crude product;
2) get normal hexane, ethyl acetate, methyl alcohol, water mixing, get and fill with mutually the high speed adverse current chromatogram post, rotate main frame, pump into the lower moving phase of doing mutually, moving phase is dissolved crude product by the sampling valve sample introduction, the UV-detector on-line monitoring, collect target component, merge the flow point drying under reduced pressure and get the high purity Tricin.
Step 1) the ethanolic soln gradient elution in is: 4-5BV40-50% ethanol elution impurity, use again 70% ethanol elution.
Step 2) normal hexane in, ethyl acetate, methyl alcohol, water blending ratio are 4-7: 5-8: 3-5: 4-6.
Technical superiority of the present invention is the preparation of process using high speed adverse current chromatogram, is the high efficiency method that a kind of yield is high, preparation amount is large, preparation cycle is short, has solved the low and with serious pollution technological deficiency of silicagel column efficient.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to the following example.
Embodiment
Embodiment 1:
The Alfalfa drying and crushing, get 1kg and add 8 times of amount 80% alcohol reflux 2 times, extracting solution is concentrated into without alcohol, add the absorption of 200ml polyamide resin column, get 5BV40% ethanolic soln wash-out impurity, use again 70% ethanolic soln wash-out, thin layer detects, it is concentrated to collect the high density flow point, and concentrated solution adds the equal-volume ethyl acetate extraction 3 times, reclaims ethyl acetate and gets crude product 8g.Get normal hexane, ethyl acetate, methyl alcohol, water by 5: 7: 4: 6 mix, and behind the standing demix, get and fill with mutually the high speed adverse current chromatogram post, rotate main frame, speed adjustment 700rpm pumps into the lower moving phase of doing mutually, after setting up running balance, flow rate regulation is 3ml/min, and simultaneously moving phase dissolving crude product is by the sampling valve sample introduction, the UV-detector on-line monitoring, collect target component, merge the flow point drying under reduced pressure, get the 910mg yellow powder, detect content 98.7% through HPLC.
Embodiment 2:
The Alfalfa drying and crushing, get 1kg and add 5 times of amount 60% alcohol reflux 3 times, extracting solution is concentrated into without alcohol, add the absorption of 250ml polyamide resin column, get 4BV50% ethanolic soln wash-out impurity, use again 70% ethanolic soln wash-out, thin layer detects, it is concentrated to collect the high density flow point, and concentrated solution adds the equal-volume ethyl acetate extraction 3 times, reclaims ethyl acetate and gets crude product 10g.Get normal hexane, ethyl acetate, methyl alcohol, water by 4: 5: 3: 4 mix, and behind the standing demix, get and fill with mutually the high speed adverse current chromatogram post, rotate main frame, speed adjustment 800rpm pumps into the lower moving phase of doing mutually, after setting up running balance, flow rate regulation is 2ml/min, and simultaneously moving phase dissolving crude product is by the sampling valve sample introduction, the UV-detector on-line monitoring, collect target component, merge the flow point drying under reduced pressure, get the 840mg yellow powder, detect content 98.2% through HPLC.
Embodiment 3:
The Alfalfa drying and crushing, get 1kg and add 7 times of amount 70% alcohol reflux 2 times, extracting solution is concentrated into without alcohol, add the absorption of 200ml polyamide resin column, get 4BV50% ethanolic soln wash-out impurity, use again 70% ethanolic soln wash-out, thin layer detects, it is concentrated to collect the high density flow point, and concentrated solution adds the equal-volume ethyl acetate extraction 3 times, reclaims ethyl acetate and gets crude product 7g.Get normal hexane, ethyl acetate, methyl alcohol, water by 7: 8: 5: 6 mix, and behind the standing demix, get and fill with mutually the high speed adverse current chromatogram post, rotate main frame, speed adjustment 700rpm pumps into the lower moving phase of doing mutually, after setting up running balance, flow rate regulation is 1ml/min, and simultaneously moving phase dissolving crude product is by the sampling valve sample introduction, the UV-detector on-line monitoring, collect target component, merge the flow point drying under reduced pressure, get the 780mg yellow powder, detect content 98.1% through HPLC.
Claims (3)
1. method of extracting Tricin from alfalfa is characterized in that following steps:
1) alfalfa is pulverized, and adds 5-8 and doubly measures the 60-80% alcohol reflux 2-3 time, and extracting solution is concentrated into without alcohol, add in the polyamide resin and adsorb, the ethanolic soln gradient elution, thin layer detects, add ethyl acetate extraction after collection high density flow point is concentrated, reclaim ethyl acetate and get crude product;
2) get normal hexane, ethyl acetate, methyl alcohol, water mixing, get and fill with mutually the high speed adverse current chromatogram post, rotate main frame, pump into the lower moving phase of doing mutually, moving phase is dissolved crude product by the sampling valve sample introduction, the UV-detector on-line monitoring, collect target component, merge the flow point drying under reduced pressure and get the high purity Tricin.
2. from alfalfa, extract as claimed in claim 1 the method for Tricin, it is characterized in that described step 1) in the ethanolic soln gradient elution be: 4-5BV40-50% ethanol elution impurity, use again 70% ethanol elution.
3. from alfalfa, extract as claimed in claim 1 the method for Tricin, it is characterized in that described step 2) in normal hexane, ethyl acetate, methyl alcohol, water blending ratio be 4-7: 5-8: 3-5: 4-6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2011102186872A CN102911146A (en) | 2011-08-02 | 2011-08-02 | Method for extracting tricin from alfalfa |
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| CN2011102186872A CN102911146A (en) | 2011-08-02 | 2011-08-02 | Method for extracting tricin from alfalfa |
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| CN102911146A true CN102911146A (en) | 2013-02-06 |
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| CN2011102186872A Pending CN102911146A (en) | 2011-08-02 | 2011-08-02 | Method for extracting tricin from alfalfa |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105497622A (en) * | 2015-12-24 | 2016-04-20 | 杭州研谱科技有限公司 | Method for extracting tricin from corn bracts |
| CN113875844A (en) * | 2021-09-29 | 2022-01-04 | 武夷山成隆天创茶业科技股份有限公司 | Application of spartina alterniflora extract in plant-derived functional tea product and functional tea product |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045720A (en) * | 2007-03-20 | 2007-10-03 | 陕西师范大学 | Method for extracting buckwheat flavone from buckwheat shell |
| CN101735189A (en) * | 2009-12-11 | 2010-06-16 | 林新华 | Preparation method, preparation and application of tricin |
| CN102040578A (en) * | 2010-12-27 | 2011-05-04 | 国际竹藤网络中心 | Method for preparing high purity tricin from bamboo leaves |
| CN102141558A (en) * | 2010-12-27 | 2011-08-03 | 国际竹藤网络中心 | Determination method for content of flavone in bamboo leaf extractive and product of bamboo leaf extractive |
-
2011
- 2011-08-02 CN CN2011102186872A patent/CN102911146A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045720A (en) * | 2007-03-20 | 2007-10-03 | 陕西师范大学 | Method for extracting buckwheat flavone from buckwheat shell |
| CN101735189A (en) * | 2009-12-11 | 2010-06-16 | 林新华 | Preparation method, preparation and application of tricin |
| CN102040578A (en) * | 2010-12-27 | 2011-05-04 | 国际竹藤网络中心 | Method for preparing high purity tricin from bamboo leaves |
| CN102141558A (en) * | 2010-12-27 | 2011-08-03 | 国际竹藤网络中心 | Determination method for content of flavone in bamboo leaf extractive and product of bamboo leaf extractive |
Non-Patent Citations (3)
| Title |
|---|
| JULIANA HWANG等: "Soy and Alfalfa Phytoestrogen Extracts Become Potent Low-Density Lipoprotein Antioxidants in the Presence of Acerola Cherry Extract", 《JOURNAL OF AGRICULTURE FOOD AND CHEMISTRY》 * |
| 何春年等: "紫花苜蓿黄酮类化学成分的研究", 《中草药》 * |
| 高蕾等: "高速逆流色谱快速分离四种甘草黄酮及其结构鉴定", 《四川化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105497622A (en) * | 2015-12-24 | 2016-04-20 | 杭州研谱科技有限公司 | Method for extracting tricin from corn bracts |
| CN113875844A (en) * | 2021-09-29 | 2022-01-04 | 武夷山成隆天创茶业科技股份有限公司 | Application of spartina alterniflora extract in plant-derived functional tea product and functional tea product |
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Application publication date: 20130206 |