CN1513822A - Technology of extracting high purity resveratrol from polygonoum cuspidatum - Google Patents
Technology of extracting high purity resveratrol from polygonoum cuspidatum Download PDFInfo
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- CN1513822A CN1513822A CNA021399115A CN02139911A CN1513822A CN 1513822 A CN1513822 A CN 1513822A CN A021399115 A CNA021399115 A CN A021399115A CN 02139911 A CN02139911 A CN 02139911A CN 1513822 A CN1513822 A CN 1513822A
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Abstract
A process for extracting high-purity resveratrol from giant knotweed rhizome includes adding special microbe for bioconversion to increase the content of resveratrol in giant knotweed rhizome, and microwave extracting in the mixture of alcohol solution and 4-methyl-2-pentanol. Its advantages are short time, low cost, and high output rate and purity.
Description
Technical field the present invention relates to active ingredients of plants and extracts the field, and a kind of technology of extracting trans-resveratrol from giant knotweed particularly is provided.
Background technology giant knotweed (Polygonum cuspidatum Sie bet Zucc) is a polygonaceae Polygonum undershrub, is China's traditional Chinese medicine.Modern pharmacy studies have shown that its resveratrol (Resveratrol) (3,4 ', 5 trihydroxy-toluylene) has anticancer, multiple pharmacological effect such as treatment cardiovascular disorder etc.
Look into new discovery, document and the patent about " extracting trans-resveratrol from giant knotweed " aspect has report both at home and abroad.Chinese patent CN1251363 and the disclosed extraction process of French Patent FR2795964 are: add prozyme in Powdered giant knotweed raw material, under constant temperature, carry out enzyme digestion reaction, obtained the enzymolysis raw material in 48--72 hour, with solvent extraction, the concentrated work in-process that obtain to contain trans-resveratrol, put 24--120 hour, and stir again, use ethyl acetate extraction then, reclaim ethyl acetate, through being further purified processing, make trans-resveratrol and polidatin again." Chemical Composition of giant knotweed, pharmacological action and the extraction separation " that " Tianjin pharmacy " delivered (1999-11-03) disclosed technology is with polygoni cuspidati,radix meal alcohol reflux, reclaim ethanol to the medicinal extract shape, be dissolved in water, filter, water liquid concentrates, concentrated solution polymeric amide chromatography obtains polidatin with 20% ethanol elution again.The people's such as Yao Baoshu that " Tianjin Light Industry College journal " (1999-04) delivered paper has been introduced and extracted Study of Resveratrol from grape skin; With organic solvent extraction that can be miscible with water, the underpressure distillation concentrated extracting solution adds distilled water to Chinese patent CN1341587 again, transfers pH to 7.5-8.0, and is concentrated with ethyl acetate extraction and underpressure distillation again with the giant knotweed powder; Chinese patent CH1239141 has introduced a kind of from grape stem, root, leaf extraction trans-resveratrol product.
Below as can be known, the processing method of existing extraction trans-resveratrol is more, but generally speaking, the existing equal technology of technology is outmoded relatively, and the production cycle is long, cost height, product yield and of low quality, complex operation.
Summary of the invention is for overcoming above-mentioned shortcoming, the invention provides a kind of technology of from giant knotweed, extracting trans-resveratrol, it has been adopted the high-performance bio transformation technology and has improved the giant knotweed Resveratrol content, utilize microwave low temperature, rapid extraction technology, technology and schedule of operation have been simplified, shorten the production cycle, reduced production cost, improved quality product.
For achieving the above object, processing step of the present invention comprises:
(1) earlier dry giant knotweed rhizome is pulverized, crossed 80 mesh sieves, add the Resveratrol Inducing agent, this inductor is a special microorganism, cultivates in optimum temperature range, makes the giant knotweed resveratrol analogs be converted into trans-resveratrol;
(2) with 40% ethanol and hydrocarbon alcohol mixed solvent microwave extracting 0.5-1 hour;
(3) centrifuging under proper temperature, concentrates under certain vacuum tightness then.
(4) column chromatography for separation concentrates, and crystallization gets the trans-resveratrol of purity 〉=95% and the by product Schuttgelb of certain purity at last.
Extracting the solvent strength ratio has a significant impact extraction efficiency, through repetition test, microwave extracting optimum condition of the present invention is: extraction solvent component volume ratio is 40% ethanol: hydrocarbon alcohol=95: 5, microwave frequency are 3000-2000MHz, 30-60 minute extraction time, 40 ℃-60 ℃ of temperature.
Invert point and time are very big to Resveratrol content raising influence in the giant knotweed, and the bio-transformation optimum temperuture is 15 ℃-45 ℃ among the present invention, and the time is 24-84 hour.
Temperature has a significant impact the stability of trans-resveratrol when concentrating, and the present invention determines that concentrating optimum temps is 45 ℃-60 ℃, vacuum tightness≤-65cmHg.
The present invention adopts the high-performance bio transformation technology, and Resveratrol content 10-20 doubly in the raising giant knotweed materials.Simultaneously, adopt microwave extraction method, compare with conventional solvent-extraction process, shortened extraction time greatly, and extraction efficiency height, avoid the labile deficiency of trans-resveratrol in the conventional solvent extraction, adopted separation, purification techniquess such as chromatography, crystallization simultaneously, obtained trans-resveratrol and two kinds of products of certain purity by product Schuttgelb of 〉=95%.
Appended drawings is that technical process Fig. 1 of the present invention, giant knotweed starting material clean, dry in the shade, pulverize 2, pre-treatment 3, microwave extraction 4, filtration, concentrate 5, column chromatography 6, wash-out 7, trans-resveratrol principal constituent are collected liquid 8, concentrate 9, crystallization 10, high-purity trans-resveratrol 11, drying, preserve 12, Schuttgelb
The embodiment processing step is:
(1) the giant knotweed rhizome that will dry in the shade is pulverized, and crosses 80 mesh sieves, claims the 500g Giant Knotweed Rhizome.
(2) in the 500g Giant Knotweed Rhizome, add an amount of trans-resveratrol special microorganism and make to transform inductor, cultivated 28 hours down for 30 ℃ in temperature;
(3) use 40% ethanol: solvent is extracted in 5%4-methyl-2-amylalcohol=conduct in 95: 5, uses microwave extracting, and extraction time 1 time/min * 5 times about each midfeather 10min, and stirs;
(4) centrifuging, filtered liquid 45 ℃ of-50 ℃ of temperature ,-concentrate under the 65cm Hg vacuum tightness.
(5) column chromatography for separation concentrates, crystallization, lyophilize, at last respectively the trans-resveratrol 2.51g of purity 95.1%, certain purity byproduct Schuttgelb 3.03g.
Claims (3)
1, a kind of giant knotweed extracts high-purity trans-resveratrol technology, and its processing step comprises:
(1) with after the dried giant knotweed pulverizing, carries out pre-treatment;
(2) microwave extracting;
(3) centrifuging, concentrating under reduced pressure;
(4) column chromatography for separation concentrates crystallization;
It is characterized in that,
(1) pre-treatment is adopted and add special microorganism in the giant knotweed raw material, cultivates 24-84 hour down at 15 ℃-45 ℃, and resveratrol analogs is carried out bio-transformation;
(2) extraction agent of microwave extracting adopts 40% ethanol and hydrocarbon alcohol mixed solvent;
(3) thickening temperature is 45 ℃-60 ℃, vacuum tightness≤-65cmHg.
2, giant knotweed according to claim 1 extracts high-purity trans-resveratrol technology, it is characterized in that, the bio-transformation temperature is 30 ℃.
3, giant knotweed according to claim 1 extracts trans-resveratrol technology, it is characterized in that the extraction solvent volume ratio is 40% ethanol: 5%4-methyl-2-amylalcohol=95: 5, microwave frequency 3000-2000MHz, 30 minutes extraction time, 40 ℃-60 ℃ of temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021399115A CN1513822A (en) | 2002-12-31 | 2002-12-31 | Technology of extracting high purity resveratrol from polygonoum cuspidatum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA021399115A CN1513822A (en) | 2002-12-31 | 2002-12-31 | Technology of extracting high purity resveratrol from polygonoum cuspidatum |
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| CN1513822A true CN1513822A (en) | 2004-07-21 |
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| CNA021399115A Pending CN1513822A (en) | 2002-12-31 | 2002-12-31 | Technology of extracting high purity resveratrol from polygonoum cuspidatum |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100344300C (en) * | 2004-09-29 | 2007-10-24 | 南京师范大学 | Cyclodextrin super molecular composition of Chinese medicine giant knutweed rhizome and its preparing method |
| CN101597214B (en) * | 2009-07-10 | 2012-04-25 | 山东省花生研究所 | Method for extracting resveratrol from peanut roots |
| CN102627677A (en) * | 2012-03-22 | 2012-08-08 | 聊城大学 | Method for separating and purifying monomer compounds from Rhizoma Polygoni Cuspidati |
-
2002
- 2002-12-31 CN CNA021399115A patent/CN1513822A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100344300C (en) * | 2004-09-29 | 2007-10-24 | 南京师范大学 | Cyclodextrin super molecular composition of Chinese medicine giant knutweed rhizome and its preparing method |
| CN101597214B (en) * | 2009-07-10 | 2012-04-25 | 山东省花生研究所 | Method for extracting resveratrol from peanut roots |
| CN102627677A (en) * | 2012-03-22 | 2012-08-08 | 聊城大学 | Method for separating and purifying monomer compounds from Rhizoma Polygoni Cuspidati |
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