CN101759732A - Method for preparing polydatin - Google Patents
Method for preparing polydatin Download PDFInfo
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- CN101759732A CN101759732A CN200910234067A CN200910234067A CN101759732A CN 101759732 A CN101759732 A CN 101759732A CN 200910234067 A CN200910234067 A CN 200910234067A CN 200910234067 A CN200910234067 A CN 200910234067A CN 101759732 A CN101759732 A CN 101759732A
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Abstract
The invention relates to a method for separating and extracting polydatin, which has low cost, large yield, short period and easy realization of industrialization, and comprises the following process steps: water extraction, macroporous resin adsorption, ultrafiltration, concentration and recrystallization. The invention is adopted to produce the polydatin, so that the process is simple, the energy consumption is low, the purity is high and the appearance is good.
Description
Technical field:
The present invention relates to the extraction and purification process of polygonin, particularly a kind of method of using macroporous resin and membrane technique separation and purification polygonin.
Background technology:
(Polydatin, Polydatin) another name piceid, polidatin are the active skull cap components that mainly is present in giant knotweed rhizome and the root to polygonin.
Chemical name: 3,4 '-5-Trihydroxystilbene-3-beta-D-glucopyranoside
Molecular formula: C
20H
22O
8
Molecular weight: 390.40
Physico-chemical property: white, needle-shaped crystals powder.Be soluble in methyl alcohol, ethanol, ethyl acetate, basic solution, be slightly soluble in water.Light stability is poor.
Occurring in nature, polygonaceae plant polygoni cuspidati,radix, Tuber Fleeceflower Root root, Pinaceae Picea glehnii bark, Myrtaceae eucalyptus genus etc. all contain polygonin, but content is the highest in dry giant knotweed rhizome and the root.But because place of production difference, the polygonin content in the giant knotweed also can change.Incomplete according to document, the polygonin content of various places giant knotweed is 1.00～2.58%, originates from wherein that content is 2.24% in the giant knotweed in Jiangsu.[.HPLC such as Qi Hui measures the content [J] of 4 kinds of compositions in the giant knotweed simultaneously. CHINA JOURNAL OF CHINESE MATERIA MEDICA .2006.12 (23): 2003-2005]
Problems such as the research of extracting about polygonin from giant knotweed has seen domestic a lot of report, but all exists technical process loaded down with trivial details, and the production cycle is long, and solvent species is many, toxicity is big, consumption is big." green fine chemistry industry natural product manufacturing process (the 1st collection) " as the Zhan Yixing chief editor mentioned ethanol extraction method and two kinds of methods of ultrasonic extraction of polygonin, but all used high volatility and the big sherwood oil of toxicity, is unfavorable for workers ' health; And for example people such as Liu Rui source " research of polidatin absorption property on macroporous adsorbent resin " disclosed a kind of method of producing polygonin with macroporous adsorption resin technology, but extracting solution need be placed and spend the night, and use ethanol, benzene, three kinds of solvents of ethyl acetate, carried out repeatedly extracting operation, prolonged the production cycle, industrial operability is not strong; Chinese patent CN1546503 has reported that gradient elution behind a kind of chromatography obtains the method for polygonin for another example, directly obtain product after the elutriant drying, though separated two kinds of primary products, but owing to there is not further purification operations, ethanol neither be best the polygonin extraction agent, in fact the purity of product can't ensure.
Summary of the invention:
The objective of the invention is in order to provide a kind of production technique simple, energy consumption is few, and cost is low, and polygonin purity reaches more than 98%, and yield is greater than 70%, and output is big, and product appearance is good, is easy to realize industrialized polygonin extraction process.
The object of the present invention is achieved like this:
1. water is carried: fresh giant knotweed is pulverized, added saturated limewater and extracted 1.5～2 hours, collect extracting solution, acid adjustment gets crude extract to pH=7～8;
2. macroporous resin adsorption: with above-mentioned crude extract, carry out saturated absorption by macroporous resin column, the ethanol elution polygonin is used in washing removal of impurities earlier again, the polygonin elutriant;
3. ultrafiltration: above-mentioned polygonin elutriant is removed macromole impurity by ultra-filtration membrane, get ultrafiltrated;
4. concentrate: with above-mentioned ultrafiltrated concentrating under reduced pressure, reclaim ethanol, get medicinal extract;
5. recrystallization: above-mentioned medicinal extract with re-crystallizing in ethyl acetate 3 times, is promptly got the white, needle-shaped crystals product.
The preparation method of above-mentioned polygonin is characterized in that it is 40～80 orders that described water is put forward the raw material pulverizing granularity of step.
The preparation method of above-mentioned polygonin is characterized in that described water puies forward condition and be: extract 6～8 times of amount saturated limewaters with raw material weight, stirring is carried out, and temperature is controlled at 50～80 ℃, extracts 1.5～2 hours.
The preparation method of above-mentioned polygonin is characterized in that described water proposes in the step acid adjustment and can select hydrochloric acid, phosphoric acid, sulfuric acid for use, and the acid adjustment terminal point is pH=7～8.
The preparation method of above-mentioned polygonin is characterized in that described macroporous resin can select D101 type, HPD-100 type, XAD-2 type macroporous resin for use.
The preparation method of above-mentioned polygonin is characterized in that the wash-out of described macroporous resin is washed macroporous resin column to colourless with deionized water earlier, uses 30～40% ethanol elution polygonins of 5～6 times of amounts of column volume again.
The preparation method of above-mentioned polygonin is characterized in that it is 500～2000 hollow fiber ultrafiltration membrane system that molecular weight cut-off is selected in described ultrafiltration for use.
The preparation method of above-mentioned polygonin is characterized in that described enrichment step solution concentration is to 1/20～1/10 of original volume.
The preparation method of above-mentioned polygonin is characterized in that described recrystallization process is as follows: the saturated dissolving of ethyl acetate normal temperature of the medicinal extract after will concentrating, and the reduction vaporization crystallization leaches crystal; Crystal is according to above-mentioned condition recrystallization 2 times.
There is following advantage in the present invention: whole process does not have heating operation except water is carried, so energy consumption is low.Utilize polygonin to be soluble in buck, be slightly soluble in the character of neutral water, just can control the dissolving of polygonin effectively and separate out, and the organic impurity of introducing is in macroporous resin adsorption with can be not residual after washing, thereby can not influence product purity by regulating pH.Water-soluble impurity had both been removed in the washing of macroporous resin, had also played decolorizing effect simultaneously, was that product appearance is better.The relative ethanol of ethyl acetate has better solvability to polygonin, as crystallizing agent the yield of polygonin and purity all is guaranteed.
So production technique of the present invention is simple, energy consumption is few, and cost is low, and polygonin purity reaches more than 98%, and yield is greater than 70%, and output is big, and the cycle is short, and product appearance is good, is easy to realize industrialization.
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:
Get the fresh giant knotweed of 10kg (polygonin content 2.13%), pulverizing in pulverizer is 40 orders, adds the 60L saturated limewater, is heated to 50 ℃, stirs and extracts 1.5 hours.With regulating pH with hydrochloric acid behind the extracting solution suction filtration is 7, gets the 65.1L crude extract.The D101 type macroporous resin saturated absorption of crude extract by column volume 5L is washed till colourlessly with deionized water, use 25L 30% ethanol elution polygonin again.The polygonin elutriant is removed macromole impurity by the hollow fiber ultrafiltration membrane system of molecular weight cut-off 500, is evaporated to 1.25L through liquid and becomes medicinal extract.Medicinal extract is with ethyl acetate saturated absorption, and decompression recrystallization 3 times finally obtains 152g content and be 99.4% polygonin white needle-like crystals.
Embodiment 2:
Get the fresh giant knotweed of 10kg (polygonin content 2.25%), pulverizing in pulverizer is 60 orders, adds the 70L saturated limewater, is heated to 70 ℃, stirs and extracts 1.75 hours.With regulating pH with phosphoric acid behind the extracting solution suction filtration is 7.3, gets the 76.4L crude extract.The HPD-100 type macroporous resin saturated absorption of crude extract by column volume 5L is washed till colourlessly with deionized water, use 28L 35% ethanol elution polygonin again.The polygonin elutriant is removed macromole impurity by the hollow fiber ultrafiltration membrane system of molecular weight cut-off 1000, is evaporated to 2L through liquid and becomes medicinal extract.Medicinal extract is with ethyl acetate saturated absorption, and decompression recrystallization 3 times finally obtains 179g content and be 98.9% polygonin white needle-like crystals.
Embodiment 3:
Get the fresh giant knotweed of 10kg (polygonin content 1.89%), pulverizing in pulverizer is 80 orders, adds the 80L saturated limewater, is heated to 80 ℃, stirs and extracts 2 hours.With regulating pH with phosphoric acid behind the extracting solution suction filtration is 8, gets the 87.6L crude extract.The XAD-2 type macroporous resin saturated absorption of crude extract by column volume 5L is washed till colourlessly with deionized water, use 30L 40% ethanol elution polygonin again.The polygonin elutriant is removed macromole impurity by the hollow fiber ultrafiltration membrane system of molecular weight cut-off 2000, is evaporated to 3L through liquid and becomes medicinal extract.Medicinal extract is with ethyl acetate saturated absorption, and decompression recrystallization 3 times finally obtains 144g content and be 98.2% polygonin white needle-like crystals.
Claims (9)
1. the preparation method of a polygonin is characterized in that comprising following step:
1. water is carried: fresh giant knotweed is pulverized, added saturated limewater and extracted 1.5～2 hours, collect extracting solution, acid adjustment gets crude extract to pH=7～8;
2. macroporous resin adsorption: with above-mentioned crude extract, carry out saturated absorption by macroporous resin column, the ethanol elution polygonin is used in washing removal of impurities earlier again, the polygonin elutriant;
3. ultrafiltration: above-mentioned polygonin elutriant is removed macromole impurity by ultra-filtration membrane, get ultrafiltrated;
4. concentrate: with above-mentioned ultrafiltrated concentrating under reduced pressure, reclaim ethanol, get medicinal extract;
5. recrystallization: above-mentioned medicinal extract with re-crystallizing in ethyl acetate 3 times, is promptly got the white, needle-shaped crystals product.
2. according to the preparation method of the described polygonin of claim 1, it is characterized in that it is 40～80 orders that described water is put forward the raw material pulverizing granularity of step.
3. according to the preparation method of the described polygonin of claim 1, it is characterized in that described water puies forward condition and be: extract 6～8 times of amount saturated limewaters with raw material weight, stirring is carried out, and temperature is controlled at 50～80 ℃, extracts 1.5～2 hours.
4. according to the preparation method of the described polygonin of claim 1, it is characterized in that described water proposes in the step acid adjustment and can select hydrochloric acid, phosphoric acid, sulfuric acid for use, the acid adjustment terminal point is pH=7～8.
5. according to the preparation method of the described polygonin of claim 1, it is characterized in that described macroporous resin can select D101 type, HPD-100 type, XAD-2 type macroporous resin for use.
6. according to the preparation method of the described polygonin of claim 1, it is characterized in that the wash-out of described macroporous resin is washed macroporous resin column to colourless with deionized water earlier, use 30～40% ethanol elution polygonins of 5～6 times of amounts of column volume again.
7. according to the preparation method of the described polygonin of claim 1, it is characterized in that it is 500～2000 hollow fiber ultrafiltration membrane system that molecular weight cut-off is selected in described ultrafiltration for use.
8. according to the preparation method of the described polygonin of claim 1, it is characterized in that described enrichment step solution concentration is to 1/20～1/10 of original volume.
9. according to the preparation method of the described polygonin of claim 1, it is characterized in that described recrystallization process is as follows: the saturated dissolving of ethyl acetate normal temperature of the medicinal extract after will concentrating, the reduction vaporization crystallization leaches crystal; Crystal is according to above-mentioned condition recrystallization 2 times.
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| CN200910234067A CN101759732A (en) | 2009-11-20 | 2009-11-20 | Method for preparing polydatin |
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| CN200910234067A CN101759732A (en) | 2009-11-20 | 2009-11-20 | Method for preparing polydatin |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344472A (en) * | 2010-08-06 | 2012-02-08 | 苏州瑞蓝博中药技术开发有限公司 | Piceid extraction technology |
| CN102453059A (en) * | 2010-10-17 | 2012-05-16 | 陕西理工学院 | Method for extracting polydatin from giant knotweed with inorganic solvent |
| CN102718811A (en) * | 2012-05-22 | 2012-10-10 | 中国人民解放军第四军医大学 | Preparation method of stilbene glycoside in polygonum cuspidatum |
| CN104004035A (en) * | 2014-06-19 | 2014-08-27 | 昆明制药集团股份有限公司 | Preparation method for 5[(2E)-(3,5-dihydroxy phenyl)ethenyl]-2-methoxyphenyl-1-O-beta-D-glucopyranoside |
| CN105777496A (en) * | 2016-03-08 | 2016-07-20 | 陈爱华 | Method for extracting resveratrol from rhizoma polygoni cuspidate and rhizoma polygoni cuspidate healthcare product |
| CN107281270A (en) * | 2016-03-30 | 2017-10-24 | 中国医学科学院药物研究所 | Application of the mulberries extract in prevention and treatment PM2.5 Lung Injury medicines are prepared |
| CN107281276A (en) * | 2016-03-30 | 2017-10-24 | 中国医学科学院药物研究所 | Application of the Gentrin Knotweed P.E in prevention and treatment PM2.5 Lung Injury medicines are prepared |
| CN107281330A (en) * | 2016-03-30 | 2017-10-24 | 中国医学科学院药物研究所 | Application of the grape skin extract in prevention and treatment PM2.5 Lung Injury medicines are prepared |
| CN108440616A (en) * | 2018-05-30 | 2018-08-24 | 云南海沣药业有限公司 | A kind of extraction separation method of polygonin |
| CN109988203A (en) * | 2017-12-31 | 2019-07-09 | 中国医学科学院药物研究所 | Polygonin crystalline substance IV type substance and preparation method and its pharmaceutical composition and purposes |
| CN110684058A (en) * | 2019-10-18 | 2020-01-14 | 江苏省中医药研究院 | Extraction equipment and extraction method of polydatin |
| CN113336805A (en) * | 2021-06-07 | 2021-09-03 | 湖南绿蔓生物科技股份有限公司 | Extraction and purification method of polydatin |
-
2009
- 2009-11-20 CN CN200910234067A patent/CN101759732A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344472A (en) * | 2010-08-06 | 2012-02-08 | 苏州瑞蓝博中药技术开发有限公司 | Piceid extraction technology |
| CN102453059A (en) * | 2010-10-17 | 2012-05-16 | 陕西理工学院 | Method for extracting polydatin from giant knotweed with inorganic solvent |
| CN102718811A (en) * | 2012-05-22 | 2012-10-10 | 中国人民解放军第四军医大学 | Preparation method of stilbene glycoside in polygonum cuspidatum |
| CN104004035A (en) * | 2014-06-19 | 2014-08-27 | 昆明制药集团股份有限公司 | Preparation method for 5[(2E)-(3,5-dihydroxy phenyl)ethenyl]-2-methoxyphenyl-1-O-beta-D-glucopyranoside |
| CN104004035B (en) * | 2014-06-19 | 2016-09-21 | 昆药集团股份有限公司 | The preparation method of 5-[(2E)-(3,5-dihydroxy phenyl) vinyl]-2-methoxyphenyl-1-O-β-D-pyranglucoside |
| CN105777496A (en) * | 2016-03-08 | 2016-07-20 | 陈爱华 | Method for extracting resveratrol from rhizoma polygoni cuspidate and rhizoma polygoni cuspidate healthcare product |
| CN107281270A (en) * | 2016-03-30 | 2017-10-24 | 中国医学科学院药物研究所 | Application of the mulberries extract in prevention and treatment PM2.5 Lung Injury medicines are prepared |
| CN107281276A (en) * | 2016-03-30 | 2017-10-24 | 中国医学科学院药物研究所 | Application of the Gentrin Knotweed P.E in prevention and treatment PM2.5 Lung Injury medicines are prepared |
| CN107281330A (en) * | 2016-03-30 | 2017-10-24 | 中国医学科学院药物研究所 | Application of the grape skin extract in prevention and treatment PM2.5 Lung Injury medicines are prepared |
| CN109988203A (en) * | 2017-12-31 | 2019-07-09 | 中国医学科学院药物研究所 | Polygonin crystalline substance IV type substance and preparation method and its pharmaceutical composition and purposes |
| CN108440616A (en) * | 2018-05-30 | 2018-08-24 | 云南海沣药业有限公司 | A kind of extraction separation method of polygonin |
| CN108440616B (en) * | 2018-05-30 | 2021-03-26 | 云南海沣药业有限公司 | Extraction and separation method of polydatin |
| CN110684058A (en) * | 2019-10-18 | 2020-01-14 | 江苏省中医药研究院 | Extraction equipment and extraction method of polydatin |
| CN113336805A (en) * | 2021-06-07 | 2021-09-03 | 湖南绿蔓生物科技股份有限公司 | Extraction and purification method of polydatin |
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Application publication date: 20100630 |