CN101805322A - Method for preparing taxifolin from fruit of princesplume ladysthumb - Google Patents
Method for preparing taxifolin from fruit of princesplume ladysthumb Download PDFInfo
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- CN101805322A CN101805322A CN201010156122A CN201010156122A CN101805322A CN 101805322 A CN101805322 A CN 101805322A CN 201010156122 A CN201010156122 A CN 201010156122A CN 201010156122 A CN201010156122 A CN 201010156122A CN 101805322 A CN101805322 A CN 101805322A
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Abstract
The invention belongs to the traditional Chinese medicine field and provides a method for preparing taxifolin from fruit of princesplume ladysthumb. The method concretely includes that: dilute alcohol crushing extraction is adopted, extract is subject to centrifugation and then is put on chromatographic column, firstly water is used for washing impurities away, then ethanol is used for eluting, eluent is destained by active carbon, destaining solution is put on chromatographic column again, chloroform-ethanol is used for eluting, reduced pressure concentration, recrystallization and drying are carried out, and clear crystal is obtained. The invention has the characteristics that crushing extraction is adopted, speed is fast, the process is safe, and a lot of time can be saved.
Description
Technical field:
The present invention relates to technical field of traditional Chinese medicines, is a kind of method for preparing Taxifolin from Princes-feather Fruit.
Background technology:
Taxifolin has another name called Taxifolin, and Taxifolin is a kind of flavanone kind composition, and chemistry is called 5,7,3 ', 4 '-tetrahydroxy flavanonol.
Molecular formula: C
15H
12O
7Molecular weight: 304.25;
Molecular structure:
Physico-chemical property: be colourless needle crystal, fusing point 208-210 ℃.Be soluble in ethanol, acetate, boiling water, be dissolved in cold water slightly, be dissolved in benzene hardly.
The Chinese medicine Princes-feather Fruit is a polygonaceae plant smartweed Polygonum orentaleL. dry mature fruit, mainly contains flavones ingredient, has diffusing Xue Xiao Disorder, the long-pending lenitive effect that disappears, Yong in Zhi Liao Disorder lump in the abdomen lump in the abdomen, goiter and tumor swell and ache, dyspepsia do not disappear the gastral cavilty distending pain.
Taxifolin can be by the activity influence lipid metabolism of regulatory enzyme; To Molt-4 and common lymphocytic propagation generation inhibition in various degree, but non-malignant cell M-9 there is not influence, for treatment malignant lymphatic cytopathy provides possibility; Can slightly suppress Squamous Cell Carcinoma (HTB43) growth; Viral enzyme had certain restraining effect; Can effectively suppress the MC lipid peroxidation of Mouse Liver.The anti-oxidation characteristics of Taxifolin and biological activity can make it be used for foodstuff additive, can be used for oxidative stress class disease at pharmaceutical field.Therefore Taxifolin has broad application prospects at food, medicine and industrial circle.
Still do not have at present the report of Taxifolin extraction process aspect at home and abroad, the present invention has filled up the blank of this respect, and the preparation method is quick, safety.
Summary of the invention:
The purpose of this invention is to provide the method for preparing Taxifolin in a kind of Princes-feather Fruit, be to be raw material with the Princes-feather Fruit medicinal material, according to the polarity and the solvability of Taxifolin,, centrifugal with broken the extraction 5-20 minute of the doubly rare alcohol of 5-15,2-4 time repeatedly, centrifugate is merged upward macroporous adsorptive resins, and first water wash-out impurity is used the 50-80% ethanol elution again, after heating, elutriant adds activated carbon decolorizing, filter, the filtrate reconcentration becomes medicinal extract, and medicinal extract and column packing are mixed the sample drying, the good chromatography column of pre-treatment on the dry method, chloroform-ethanol elution, collect elutriant, concentrating under reduced pressure reclaims solvent, benzene-ethyl alcohol recrystallization, low temperature growing the grain, filtration drying promptly get product.
Described medicinal material Princes-feather Fruit is chosen the Princes-feather Fruit that late September to early November gathers, the Princes-feather Fruit that gather preferred mid-October.
Described rare alcohol is the ethanolic soln of concentration 35-55%.
Described centrifugally operated speed control is at 3000-5000r/min, time 8-15 minute.
Described macroporous resin is selected low-pole or Semi-polarity macroporous resin for use, and as AB-8, HPD300, NKA-9 etc., water elution trash flow speed control is built in 1-3BV/h, the wash-out consumption is 4-6BV, and the ethanol elution speed control is at 2-6BV/h, and the thin layer inspection is known, be eluted to no Taxifolin flow point, collect this section flow point.
The optional polyamide resin of described chromatography column filler, dextrane gel, preferred dextrane gel, the eluent chloroform: proportion of ethanol is 4: 1-10: 1, elution speed 1.5-4BV/h, preferred 2BV/h.
Recrystallization solvent for use benzene-ethanol volume ratio is 1: 1, growing the grain temperature-4-5 ℃, and recrystallization 2-5 time.
The present invention has the following advantages:
1) the present invention serves as to extract solvent with rare alcohol, and inexpensive nontoxic, crush method is extracted fast, safety, and the Taxifolin of extraction is easy to decolouring, crystallization.
2) the present invention adopts macroporous resin in conjunction with polymeric amide or sephadex column, good separating effect, product purity height.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Water intaking Safflower fruit medicinal material 10g, being placed on crusher in crushing with the 60mL50% alcohol immersion extracted 15 minutes, extract is put into whizzer, under the 3000r/min condition centrifugal 10 minutes, repetitive operation 3 times merged centrifugate, with HPD300 macroporous resin on the centrifugate, with 5 times of column volume water elution impurity, flow velocity 1.5BV/h knows no Taxifolin flow point with 60% ethanol elution to thin layer inspection more earlier, collect the Taxifolin flow point, heating adds gac constant temperature again to 60 ℃ and stirs decolouring 1h, filters, and filtrate is condensed into medicinal extract, medicinal extract and dextrane gel are mixed after the sample drying Sephadex LH-20 post on the dry method, chloroform-ethanol (6: 1) wash-out, flow velocity 4BV/h, the thin layer inspection is known, collect the Taxifolin flow point, concentrating under reduced pressure reclaims solvent, crude product, benzene-ethanol (1: 1) saturated dissolving that refluxes, cool off 0 ℃ and leave standstill crystallization, recrystallization 2 times filters, and vacuum-drying gets purity at 98% Taxifolin crystal 7.9mg.
Embodiment 2:
Water intaking Safflower fruit medicinal material 10g, being placed on crusher in crushing with the 100mL45% alcohol immersion extracted 20 minutes, extract is put into whizzer, under the 3500r/min condition centrifugal 15 minutes, repetitive operation 2 times merges centrifugate, with NKA-9 macroporous resin on the centrifugate, earlier with 4 times of column volume water elution impurity, flow velocity 2BV/h knows no Taxifolin flow point with 50% ethanol elution to thin layer inspection again, collects the Taxifolin flow point, heat and add gac constant temperature again to 60 ℃ and stir decolouring 1h, filter, filtrate is condensed into medicinal extract, and medicinal extract and dextrane gel are mixed after the sample drying Sephadex LH-20 post on the dry method, chloroform-ethanol (9: 1) wash-out, the inspection of flow velocity 4BV/h thin layer is known, and collects the Taxifolin flow point, and concentrating under reduced pressure reclaims solvent, get crude product, benzene-ethanol (1: 1) saturated dissolving that refluxes is cooled off-4 ℃ and is left standstill crystallization, recrystallization 5 times, filter, vacuum-drying gets purity at 98.8% Taxifolin crystal 11.2mg.
Embodiment 3:
Water intaking Safflower fruit medicinal material 20g, being placed on crusher in crushing with the 240mLA0% alcohol immersion extracted 10 minutes, extract is put into whizzer, under the 4000r/min condition centrifugal 12 minutes, repetitive operation 3 times merged centrifugate, with HPD600 macroporous resin on the centrifugate, with 5 times of column volume water elution impurity, flow velocity 3BV/h knows no Taxifolin flow point with 75% ethanol elution to thin layer inspection more earlier, collect the Taxifolin flow point, heating adds gac constant temperature again to 60 ℃ and stirs decolouring 1h, filters, and filtrate is condensed into medicinal extract, medicinal extract and dextrane gel are mixed after the sample drying Sephadex LH-20 post on the dry method, chloroform-ethanol (5: 1) wash-out, flow velocity 1.5BV/h, the thin layer inspection is known, collect the Taxifolin flow point, concentrating under reduced pressure reclaims solvent, crude product, benzene-ethanol (1: 1) saturated dissolving that refluxes, cool off 5 ℃ and leave standstill crystallization, recrystallization 3 times filters, and vacuum-drying gets purity at 98.5% Taxifolin crystal 16.5mg.
Embodiment 4:
Water intaking Safflower fruit medicinal material 50g, being placed on crusher in crushing with the 750mL50% alcohol immersion extracted 18 minutes, extract is put into whizzer, under the 5000r/min condition centrifugal 8 minutes, repetitive operation 2 times merged centrifugate, with AB-8 macroporous resin on the centrifugate, with 6 times of column volume water elution impurity, flow velocity 1BV/h knows no Taxifolin flow point with 80% ethanol elution to thin layer inspection more earlier, collect the Taxifolin flow point, heating adds gac constant temperature again to 60 ℃ and stirs decolouring 1h, filters, and filtrate is condensed into medicinal extract, medicinal extract and polyamide resin are mixed after the sample drying Sephadex LH-20 post on the dry method, chloroform-ethanol (4: 1) wash-out, flow velocity 3BV/h, the thin layer inspection is known, collect the Taxifolin flow point, concentrating under reduced pressure reclaims solvent, crude product, benzene-ethanol (1: 1) saturated dissolving that refluxes, cool off 2 ℃ and leave standstill crystallization, recrystallization 4 times filters, and vacuum-drying gets purity at 99% Taxifolin crystal 4 2.7mg.
Claims (6)
1. method that from Princes-feather Fruit, prepares Taxifolin, the its preparation method process is as follows: with the Princes-feather Fruit medicinal material is raw material, according to the polarity and the solvability of Taxifolin,, centrifugal with broken the extraction 5-20 minute of the doubly rare alcohol of 5-15, repeat 2-4 time, centrifugate is merged upward macroporous adsorptive resins, and first water wash-out impurity is used the 50-80% ethanol elution again, after heating, elutriant adds activated carbon decolorizing, filter, the filtrate reconcentration becomes medicinal extract, and medicinal extract and column packing are mixed the sample drying, the good chromatography column of pre-treatment on the dry method, chloroform-ethanol elution, collect elutriant, concentrating under reduced pressure reclaims solvent, benzene-ethyl alcohol recrystallization, low temperature growing the grain, filtration drying promptly get product.
2. the method for preparing Taxifolin according to claim 1 is characterized in that described medicinal material Princes-feather Fruit chooses the Princes-feather Fruit that late September to early November gathers.
3. the method for preparing Taxifolin according to claim 1 is characterized in that described centrifugally operated speed control at 3000-5000r/min, time 8-15 minute.
4. the method for preparing Taxifolin according to claim 1, it is characterized in that macroporous resin selects low-pole or Semi-polarity macroporous resin for use, as AB-8, HPD300, NKA-9 etc., water elution trash flow speed control is built in 1-3BV/h, the wash-out consumption is 4-6BV, and the ethanol elution speed control is at 2-6BV/h, and the thin layer inspection is known, be eluted to no Taxifolin flow point, collect this section flow point.
5. the method for preparing Taxifolin according to claim 1 is characterized in that the optional polyamide resin of chromatography column filler, dextrane gel, the eluent chloroform: proportion of ethanol is 4: 1-10: 1, and elution speed 1.5-4BV/h.
6. the method for preparing Taxifolin according to claim 1 is characterized in that recrystallization solvent for use benzene-ethanol volume ratio is 1: 1, growing the grain temperature-4-5 ℃, and recrystallization 2-5 time.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010156122A CN101805322A (en) | 2010-04-27 | 2010-04-27 | Method for preparing taxifolin from fruit of princesplume ladysthumb |
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| CN201010156122A CN101805322A (en) | 2010-04-27 | 2010-04-27 | Method for preparing taxifolin from fruit of princesplume ladysthumb |
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| CN101805322A true CN101805322A (en) | 2010-08-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108056349A (en) * | 2018-01-10 | 2018-05-22 | 广东日可威食品原料有限公司 | A kind of juvenile healthy weight-reducing drinks |
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2010
- 2010-04-27 CN CN201010156122A patent/CN101805322A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108056349A (en) * | 2018-01-10 | 2018-05-22 | 广东日可威食品原料有限公司 | A kind of juvenile healthy weight-reducing drinks |
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Application publication date: 20100818 |