CN102134286A - Method for extracting rhizoma anemarrhenae polysaccharide from rhizoma anemarrhenae decoction pieces - Google Patents
Method for extracting rhizoma anemarrhenae polysaccharide from rhizoma anemarrhenae decoction pieces Download PDFInfo
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- CN102134286A CN102134286A CN 201110120368 CN201110120368A CN102134286A CN 102134286 A CN102134286 A CN 102134286A CN 201110120368 CN201110120368 CN 201110120368 CN 201110120368 A CN201110120368 A CN 201110120368A CN 102134286 A CN102134286 A CN 102134286A
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Abstract
The invention discloses a method for extracting rhizoma anemarrhenae polysaccharide from rhizoma anemarrhenae decoction pieces, which comprises the following steps: removing micromolecules by conducting ethanol extraction to the rhizoma anemarrhenae decoction pieces, drying residues and extracting the residues with deionized water, merging and concentrating the extracting solution, precipitating with ethanol, conducting pumping filtering to obtain a supernatant and a filter cake, and washing the filter cake to obtain an extractum containing neutral polysaccharide N1; precipitating the supernatant with ethanol, conducting pumping filtering, washing the filter cake to obtain an extractum containing neutral polysaccharide N2; drying water extraction residues and then extracting with an alkali liquor, neutralizing the extracting solution to be neutral with hydrochloric acid, precipitating after concentration, conducting pumping filtering to obtain an upper supernatant and a filter cake, and washing the filter cake to obtain an extractum containing acid polysaccharide A1; precipitating the supernatant with ethanol, conducting pumping filtering, and washing the filter cake to obtain the extractum containing acid polysaccharide A2. The method has the advantages of utilizing the residues of the rhizoma anemarrhenae, and adopting alkali extraction on the basis of water extraction, thus improving the extraction efficiency of rhizoma anemarrhenae polysaccharide, enriching the variety of polysaccharide in rhizoma anemarrhenae, and improving the content of polysaccharide.
Description
Technical field
The present invention relates to a kind of method, belong to the anemaran technology of preparing by wind-weed medicine materical crude slice extraction anemaran.
Background technology
Polysaccharide is a class biomacromolecule material, has begun extensive studies from 20th century, studies have shown that polysaccharide has a series of pharmacologically active, as: enhance immunity power, hypoglycemic, anti-inflammatory, antitumor etc.Compare with the medicine that existing market is used, have effective, nontoxic advantage.Bibliographical information has proved that anemaran is that a class has the polysaccharide that higher pharmacology is worth, and especially the effect aspect hypoglycemic is more outstanding.Therefore extract the focus that anemaran becomes anemaran research preferably.
The wind-weed (Rhizome Anemarrnema) is the dry rhizome of the liliaceous plant wind-weed (Anemarrhenaashphodeloides Bge), and the property bitter taste is cold, has heat-clearing and fire-purging, and the effect of promoting the production of body fluid and moisturizing is a class heat-clearing and fire-purging drug commonly used.
Use for the research of the wind-weed at present, mainly concentrate on the various small molecules compositions that ethanol-extracted obtains, wherein main component contains steroid saponin, flavonoid, lignin and sterols, pharmacological actions such as that these compositions have is antitumor, reducing blood-fat, anti-senile dementia and anti-inflammatory, in the application in modern times also relatively extensively.
Existing method by wind-weed extraction anemaran only limits to the water extraction of the wind-weed, as usefulness distilled water refluxing extraction Common Anemarrhena Rhizome 1h such as Zhou Yonggang, extracting solution merges the concentrated extracting solution that promptly obtains anemaran, and the content of anemaran in the extracting solution carried out measuring (Zhou Yonggang, Bian Yanfang, Chen Wansheng. the assay of wind-weed total polysaccharides [J]. pharmacy practice magazine, 1999,17 (5): 306-307.); Guan Honghui etc. reflux Common Anemarrhena Rhizome 3 times 90 ℃ of water-baths, each 40min, merging filtrate, concentrate, four times of ethanol sedimentations have obtained general extractive (Guan Honghui, the Guo Qiuping of anemaran, Gao Ying, Deng. Mangiferin and content Determination of Polysaccharide [J] in the wind-weed in the different places of production. the time precious traditional Chinese medical science traditional Chinese medicines, 2009,20 (1): 182-184.).
The weak point of this method is that the residue after water is carried is considered as refuse and abandons, and causes the anemaran effective constituent in the residue to waste.
The present invention has been primarily aimed at the difference of the soda acid character of anemaran, adopts two kinds of solvents that the polysaccharide in the wind-weed medicine materical crude slice is extracted, and has prepared two kinds of anemarans, has enriched the kind of polysaccharide, has improved content.
Summary of the invention
The object of the invention provides a kind of method by wind-weed medicine materical crude slice extraction anemaran, and this procedure is simple, and the anemaran composition of extraction is many, widens the anemaran pharmacologically active.
The present invention is realized that by the following technical programs a kind of method by wind-weed medicine materical crude slice extraction anemaran is characterized in that, may further comprise the steps:
(1) with wind-weed medicine materical crude slice after 60～65 ℃ of dryings of temperature, pulverized 100 mesh sieves, the accurate title, decide, it is added mass concentration is that 60～80% aqueous ethanolic solutions are at 90 ℃ of refluxing extraction 1～3h of temperature, the reject extracting solution, and carry out refluxing extraction 3 times by the 1st refluxing extraction operational condition, then filtered and recycled Common Anemarrhena Rhizome residue;
(2) with step (1) Common Anemarrhena Rhizome residue in temperature 60-65 ℃ drying, mass ratio by exsiccant Common Anemarrhena Rhizome residue and deionized water is 1: (10～30), the Common Anemarrhena Rhizome residue is added in the deionized water, at 60～100 ℃ of refluxing extraction 1～3h of temperature, reclaim extracting solution, and carry out refluxing extraction 3 times by the 1st refluxing extraction operational condition, recycle-water is carried wind-weed medicine materical crude slice residue, united extraction liquid.The extracting solution that merges concentrates through reduction vaporization, 3 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, reclaim supernatant liquor, throw out washs with dehydrated alcohol, ether, wash do not have color to washings till, suction filtration, it is 40%～50% neutral polysaccharide N that the filter cake lyophilize obtains mass content
1Be main wind-weed medicinal extract;
(3) supernatant that step (2) is reclaimed concentrates through reduction vaporization, 4 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, remove supernatant liquor, throw out washs with dehydrated alcohol, ether, wash do not have color to washings till, suction filtration, it is 60%～70% neutral polysaccharide N that the filter cake lyophilize obtains mass content
2Be main wind-weed medicinal extract;
(4) water that step (2) is reclaimed is carried the Common Anemarrhena Rhizome residue after 60～65 ℃ of dryings of temperature, the ratio of carrying Common Anemarrhena Rhizome residue quality gram number and sodium hydroxide solution volume milliliter number by exsiccant water is 1: (10-30), water is carried the Common Anemarrhena Rhizome residue to add in 0.1～0.3mol/L sodium hydroxide solution, at 60～100 ℃ of refluxing extraction 1～3h of temperature, reclaim extracting solution, and carry out refluxing extraction 3 times, united extraction liquid by the 1st refluxing extraction operational condition.In united extraction liquid, drip 0.1～0.3mol/L hydrochloric acid to the pH of united extraction liquid be 6～8, concentrate through reduction vaporization, 3 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, reclaim supernatant liquor, throw out is with dehydrated alcohol, ether washing, wash do not have color to washings till, it is 30%～40% acidic polysaccharose A that suction filtration, filter cake lyophilize obtain mass content
1Be main wind-weed medicinal extract;
(5) supernatant liquor that step (4) is reclaimed concentrates through reduction vaporization, 4 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, remove supernatant liquor, throw out washs with dehydrated alcohol, ether, wash do not have color to washings till, after filtration, it is 40%～50% acidic polysaccharose A that the filter cake lyophilize obtains mass content
2Be main wind-weed medicinal extract.
The invention has the advantages that leaching process is simple, environmental protection has improved the rate of recovery of anemaran simultaneously, and the further distinct composition and the content of wind-weed total polysaccharides reaches the purpose that makes full use of and protect Chinese medicine wind-weed resource.
Description of drawings
The infrared scan figure of the anemaran that is contained in the medicinal extract that Fig. 1 is extracted for the embodiment of the invention 1, infrared curve 1 is anemaran A
1, infrared curve 2 is anemaran A
2, infrared curve 3 is anemaran N
1, infrared curve 4 is anemaran N
2
Embodiment
Example 1
Wind-weed medicine materical crude slice is dry in 60 ℃ of baking ovens, pulverize, cross 100 mesh sieves, precision takes by weighing 100g.Adding mass concentration is in 80% aqueous ethanolic solution, 90 ℃ of refluxing extraction of temperature 3 times, each 1h, the reject extracting solution, filtered and recycled wind-weed residue is in 60 ℃ of dryings of temperature (45.29g), add in the 680ml deionized water, 90 ℃ of refluxing extraction 3 times, each 1h, united extraction liquid and recycle-water are carried wind-weed residue.The extracting solution reduction vaporization adds 1200ml ethanol and stirs all to 400ml, precipitates 24h in 4 ℃ of refrigerators.Suction filtration must be gone up cleer and peaceful filter cake two portions, and supernatant liquor is standby, and filter cake washs to washings with dehydrated alcohol, ether does not have color, and the lyophilize filter cake must contain neutral polysaccharide N
1Be main wind-weed medicinal extract.It is 70ml that supernatant continues reduction vaporization to volume, and with precipitating 24h in 4 ℃ of refrigerators of 280ml ethanol, the washing lyophilize must contain neutral polysaccharide N
2Be main wind-weed medicinal extract.Water is put forward 60 ℃ of oven for drying of wind-weed residue (27.34g), adds 410ml sodium hydroxide (0.1mol/L) and extracts each 1.5h 3 times in 100 ℃.United extraction liquid is neutralized to PH=6～8 of extracting solution, reduction vaporization, the same N of intermediate processing with 0.1mol/L hydrochloric acid
1And N
2, obtain acidic polysaccharose A
1, A
2Be main wind-weed medicinal extract.Obtain neutral polysaccharide medicinal extract N altogether
1: 13g, N
2: 0.58g; The acidic polysaccharose extractum A
1: 6.8g, A
2: 0.36g.Content to polysaccharide in two types the polysaccharide medicinal extract that obtains is measured with sulfuric acid-anthrone method, and calculates the content of polysaccharide in the rhizoma ane marrhenae, result such as table 1:
The assay result of table 1 anemaran
Example 2
Wind-weed medicine materical crude slice is dry in 60 ℃ of baking ovens, pulverize, cross 100 mesh sieves, precision takes by weighing 100g.Adding mass concentration is in 70% aqueous ethanolic solution, and 90 ℃ of refluxing extraction of temperature 3 times, each 1h, reject extracting solution, filtered and recycled wind-weed residue be in 60 ℃ of oven dry (51.3582g), adds the 770ml deionized water and extracts 3 times in 90 ℃, at every turn 1h.Extracting solution merges reduction vaporization to 470ml, adds 1410ml ethanol and stirs, and precipitates 24h in 4 ℃ of refrigerators, suction filtration must be gone up cleer and peaceful filter cake two portions, supernatant liquor is standby, and filter cake washs to washings with dehydrated alcohol, ether does not have color, and the lyophilize filter cake must contain neutral polysaccharide N
1Be main wind-weed medicinal extract.Supernatant continues reduction vaporization to 88ml, and with precipitating 24h in 4 ℃ of refrigerators of 352ml ethanol, the washing lyophilize obtains neutral polysaccharide N
2Be main wind-weed medicinal extract.Water is put forward 60 ℃ of oven for drying of wind-weed residue (36.83), adds 921ml sodium hydroxide (0.1mol/L) and extracts each 1.5h 3 times in 100 ℃.United extraction liquid is neutralized to PH=6～8 with 0.1mol/L hydrochloric acid, reduction vaporization, the same N of intermediate processing
1And N
2, obtain acidic polysaccharose A
1, A
2Be main wind-weed medicinal extract.Obtain neutral polysaccharide medicinal extract N altogether
1: 13.5g, N
2: 0.55g; The acidic polysaccharose extractum A
1: 7.2g, A2:0.4g.Content to polysaccharide in two types the polysaccharide medicinal extract that obtains is measured with sulfuric acid-anthrone method, and calculates the content of polysaccharide in the rhizoma ane marrhenae, and the result is as follows:
Example 3:
Wind-weed medicine materical crude slice is dry in 60 ℃ of baking ovens, pulverize, cross 100 mesh sieves, precision takes by weighing 100g.Adding mass concentration is in 80% aqueous ethanolic solution, and 90 ℃ of refluxing extraction of temperature 2 times, each 1.5h, reject extracting solution, filtered and recycled wind-weed residue add the 955ml water extraction 2 times in 60 ℃ of oven dry (63.6271g), 1h at every turn, 90 ℃ of temperature.Extracting solution merges reduction vaporization to 290ml, adds 810ml ethanol and stirs, and precipitates 24h in 4 ℃ of refrigerators, suction filtration must be gone up cleer and peaceful filter cake two portions, supernatant liquor is standby, and filter cake washs to washings with dehydrated alcohol, ether does not have color, and lyophilize must contain neutral polysaccharide N
1It is main anemaran.Supernatant continues reduction vaporization to 47ml, and with precipitating 24h in 4 ℃ of refrigerators of 188ml ethanol, washing obtains neutral polysaccharide N
2It is main anemaran.Extract 60 ℃ of oven dry of residual residue (45.73g), add 1143ml sodium hydroxide (0.1mol/L) and extract 2 times, each 1.5h, 100 ℃ of temperature, united extraction liquid is neutralized to PH=6～8 with 0.1mol/L hydrochloric acid, concentrating under reduced pressure, the same N of intermediate processing
1And N
2, obtain acidic polysaccharose A
1, A
2It is main anemaran.Obtain neutral polysaccharide N altogether
1: 9.43g, N
2: 0.32g; Acidic polysaccharose A
1: 5.39g, A
2: 0.27g.Content to polysaccharide in two types the polysaccharide medicinal extract that obtains is measured with sulfuric acid-anthrone method, and calculates the content of polysaccharide in the rhizoma ane marrhenae, and the result is as follows:
Claims (1)
1. the method by wind-weed medicine materical crude slice extraction anemaran is characterized in that, may further comprise the steps:
(1) with wind-weed medicine materical crude slice after 60～65 ℃ of dryings of temperature, pulverized 100 mesh sieves, the accurate title, decide, it is added mass concentration is that 60～80% aqueous ethanolic solutions are at 90 ℃ of refluxing extraction 1～3h of temperature, the reject extracting solution, and carry out refluxing extraction 3 times by the 1st refluxing extraction operational condition, then filtered and recycled Common Anemarrhena Rhizome residue;
(2) with step (1) Common Anemarrhena Rhizome residue in temperature 60-65 ℃ drying, mass ratio by exsiccant Common Anemarrhena Rhizome residue and deionized water is 1: (10～30), the Common Anemarrhena Rhizome residue is added in the deionized water, at 60～100 ℃ of refluxing extraction 1～3h of temperature, reclaim extracting solution, and carry out refluxing extraction 3 times by the 1st refluxing extraction operational condition, recycle-water is carried wind-weed medicine materical crude slice residue, united extraction liquid; The extracting solution that merges concentrates through reduction vaporization, 3 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, reclaim supernatant liquor, throw out washs with dehydrated alcohol, ether, wash do not have color to washings till, suction filtration, it is 40%～50% neutral polysaccharide N that the filter cake lyophilize obtains mass content
1Be main wind-weed medicinal extract;
(3) supernatant that step (2) is reclaimed concentrates through reduction vaporization, 4 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, remove supernatant liquor, throw out washs with dehydrated alcohol, ether, wash do not have color to washings till, suction filtration, it is 60%～70% neutral polysaccharide N that the filter cake lyophilize obtains mass content
2Be main wind-weed medicinal extract;
(4) water that step (2) is reclaimed is carried the Common Anemarrhena Rhizome residue after 60～65 ℃ of dryings of temperature, the ratio of carrying Common Anemarrhena Rhizome residue quality gram number and sodium hydroxide solution volume milliliter number by exsiccant water is 1: (10-30), water is carried the Common Anemarrhena Rhizome residue to add in 0.1～0.3mol/L sodium hydroxide solution, at 60～100 ℃ of refluxing extraction 1～3h of temperature, reclaim extracting solution, and carry out refluxing extraction 3 times, united extraction liquid by the 1st refluxing extraction operational condition.In united extraction liquid, drip 0.1～0.3mol/L hydrochloric acid to the pH of united extraction liquid be 6～8, concentrate through reduction vaporization, 3 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, reclaim supernatant liquor, throw out is with dehydrated alcohol, ether washing, wash do not have color to washings till, it is 30%～40% acidic polysaccharose A that suction filtration, filter cake lyophilize obtain mass content
1Be main wind-weed medicinal extract;
(5) supernatant liquor that step (4) is reclaimed concentrates through reduction vaporization, 4 times the ethanol that in concentrated solution, adds volume, precipitate 23-25h down at temperature 3-4 ℃ then, remove supernatant liquor, throw out washs with dehydrated alcohol, ether, wash do not have color to washings till, after filtration, it is 40%～50% acidic polysaccharose A that the filter cake lyophilize obtains mass content
2Be main wind-weed medicinal extract.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191289A (en) * | 2013-04-08 | 2013-07-10 | 广州中医药大学 | Synchronous preparation method of four effective parts in medicine pair of common anemarrhena rhizome and amur corktree bark and application thereof |
| CN112876577A (en) * | 2021-03-18 | 2021-06-01 | 华南理工大学 | Homogeneous rhizoma anemarrhenae polysaccharide and preparation method and application thereof |
| CN115572318A (en) * | 2022-10-23 | 2023-01-06 | 爱生泽(上海)生物科技有限公司 | Preparation method of anemarrhena oligosaccharide and application of anemarrhena oligosaccharide in cosmetics |
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| JPS55108403A (en) * | 1979-02-13 | 1980-08-20 | Mitsubishi Chem Ind Ltd | Hypoglycemic |
| CN1555831A (en) * | 2003-12-31 | 2004-12-22 | 悦康药业集团有限公司 | Compound formula preparation eontaining glucocorticoid medicine |
| CN1562276A (en) * | 2004-03-26 | 2005-01-12 | 悦康药业集团有限公司 | Application of anemarrhena extract in preparing mediciation for preventing and curing abnormal rapidity heart rate and essential hyperension |
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2011
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Patent Citations (3)
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| JPS55108403A (en) * | 1979-02-13 | 1980-08-20 | Mitsubishi Chem Ind Ltd | Hypoglycemic |
| CN1555831A (en) * | 2003-12-31 | 2004-12-22 | 悦康药业集团有限公司 | Compound formula preparation eontaining glucocorticoid medicine |
| CN1562276A (en) * | 2004-03-26 | 2005-01-12 | 悦康药业集团有限公司 | Application of anemarrhena extract in preparing mediciation for preventing and curing abnormal rapidity heart rate and essential hyperension |
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| 《中国优秀硕士学位论文全文数据库 工程科技I辑》 20090115 吴妍 知母提取物的提取及制剂工艺研究 第6，27页 1 , * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191289A (en) * | 2013-04-08 | 2013-07-10 | 广州中医药大学 | Synchronous preparation method of four effective parts in medicine pair of common anemarrhena rhizome and amur corktree bark and application thereof |
| CN112876577A (en) * | 2021-03-18 | 2021-06-01 | 华南理工大学 | Homogeneous rhizoma anemarrhenae polysaccharide and preparation method and application thereof |
| CN112876577B (en) * | 2021-03-18 | 2022-02-22 | 华南理工大学 | Homogeneous rhizoma anemarrhenae polysaccharide and preparation method and application thereof |
| CN115572318A (en) * | 2022-10-23 | 2023-01-06 | 爱生泽(上海)生物科技有限公司 | Preparation method of anemarrhena oligosaccharide and application of anemarrhena oligosaccharide in cosmetics |
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