CN104739920A - Method for extracting total saponins of astragalus from traditional Chinese medicine astragalus - Google Patents
Method for extracting total saponins of astragalus from traditional Chinese medicine astragalus Download PDFInfo
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- CN104739920A CN104739920A CN201510172731.9A CN201510172731A CN104739920A CN 104739920 A CN104739920 A CN 104739920A CN 201510172731 A CN201510172731 A CN 201510172731A CN 104739920 A CN104739920 A CN 104739920A
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Abstract
The invention provides a method for extracting total saponins of astragalus from traditional Chinese medicine astragalus. The method comprises the following steps: performing water extraction, performing alcohol precipitation, performing alkalization, performing macroporous resin purification, standing, filtering and the like. According to the method disclosed by the invention, the problems of relatively low yield of extracting the total saponins of astragalus from traditional Chinese medicine astragalus, low content of total saponins of astragalus, relatively high production cost and the like in the prior art are solved. Three main indexes of the content of total saponins of astragalus, the methyl glycoside content and the yield are taken into consideration; and meanwhile, the load of macroporous resin is reduced, the repeated using times of the macroporous resin are increased, and the method is environmentally friendly. The content of the total saponins of astragalus is higher than 85%, the yield is about 0.10%, the content of the total saponins of astragalus is more than 60%, and the product is light in color.
Description
Technical field
The invention belongs to medical art, be specifically related to a kind of method extracting the Radix Astragali total saponins of high Astragaloside content from the Radix Astragali.
Background technology
" Chinese Pharmacopoeia " version regulation in 2010, the Radix Astragali is the dry root of leguminous plant Radix Astagali [Astragalus membranaceus (Fisch.) Bge.var.mongholicus (Bge) Hsiao] or Radix Astragali [A.membranaceus (Fisch.) Bge], has invigorating QI to consolidate the body surface resistance, the effect such as diuresis is promoted the production of body fluid, expelling pus and toxin by strengthening QI, expelling pus and promoting granulation.The main chemical compositions of the Radix Astragali has saponins, flavonoid and polysaccharide etc.Saponin component mainly contains astragaloside I ~ VIII, different astragaloside I, II, IV and Sayasaponin Ⅰ.Astragaloside (Astragaloside IV) is one of main active of Radix Astragali enhancing human body immunity function, is also the quantitative target composition containing Milkvetch Root preparation.Radix Astragali total saponins has effects such as regulating blood glucose, enhancing human body immunity, growth promoting effects and raising antioxidant ability of organism.
Summary of the invention
The object of this invention is to provide a kind of method extracting Radix Astragali total saponins from the Radix Astragali that Astragaloside content being applicable to large-scale production is high.The method technique is simple, production cost is low, productive rate purity is high and stable, and simultaneously in implementation procedure, precipitate with ethanol is precipitated as Radix Astragali crude polysaccharides, can processing and utilization further, realizes green production.
The method that Radix Astragali total saponins is prepared in extraction provided by the present invention comprises the following steps:
A, Radix Astragali crude drug add water to submerge, circumfluence distillation, and extracting solution is concentrated into thick extractum;
In this step, solubilization dosage conveniently consumption, is generally the water of 6 ~ 12 times amount.The parameter of circumfluence distillation time also conveniently in technique is carried out, and is generally 1 ~ 3 hour.
B, thick extractum add ethanol makes concentration of alcohol reach 70 ~ 90%, and be stirred to after precipitation separates out completely, filter, supernatant concentration, to clear paste, is 8 ~ 10 by aqueous slkali adjust ph, and hold over night, obtains alkali treatment liquid; Aqueous slkali in described step b is the sodium hydroxide solution of mass concentration 30 ~ 60%;
In this step, concentration of alcohol is selected can reach precipitate with ethanol object for principle.General control ethanol content 70 ~ 90%, to make the stripping of Astrageloside material, simultaneously other material sedimentations.Tannin is polyphenol derivatives, is extensively present among medical material, and its existence can have influence on the stability of later stage Radix Astragali total saponins related preparations.The sodium hydroxide solution adjust pH adding 30 ~ 60% is 8 ~ 10, can remove tannin preferably, and the retention rate of Radix Astragali total saponins is also higher.Meanwhile, basification can make the saponin such as astragaloside I, Radix Astragali saponin II, acetyl astragaloside I and different Radix Astragali saponin II under alkaline environment, be hydrolyzed deacetylation and be converted into astragaloside, thus improves output and the purity of astragaloside.
C, get alkali treatment liquid and join macroporous adsorptive resins, with the deionized-distilled water eluting carbohydrate fraction of 10 ~ 15 times of column volumes, again with 20 ~ 30% of 5-10 times of column volume ethanol elution, finally with 75 ~ 95% of 5 ~ 10 times of column volumes ethanol elution, collect high concentration ethanol eluent, add a small amount of water dissolution after concentrate drying, leave standstill 12 ~ 48 hours, filter to obtain precipitation;
The direct loading macroporous adsorptive resins of alkali treatment liquid in this step, loading volume is less and also load solution is washed till neutrality while deionized-distilled water eluting carbohydrate fraction.During low concentration alcohol eluting, alcoholic degree must lower than 30%, can effectively remove impurity, prevents again the loss of effective ingredient.High concentration alcohol higher than 75%, must contribute to the desorption of saponin, thus improves the response rate of target product.
D, taking precipitate are dried, and are Radix Astragali total saponins.In this Radix Astragali total saponins, Astragaloside content is higher.
Compared with prior art, this method obtains the load solution of macroporous resin column after first adopting the pretreatment such as water extraction, precipitate with ethanol, concentrated and alkalization, greatly reduce the consumption of water during eluting resin, decrease the load of macroporous resin, improve its repeat usage.Again load solution is adjusted to neutrality by alkalescence while water elution carbohydrate fraction, simplifies the operation and cost-saving.Target product yield prepared by the inventive method is high, Radix Astragali total saponins and Astragaloside content is high, of light color, stable yield, and without chemical agent residue, leaching process environmental friendliness, requires low to reagent facility, is applicable to large-scale industrial production.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, and embodiment is explanation of the invention instead of limiting the scope of the present invention.
Embodiment 1
To raw medicinal material prepared by Radix Astragali total saponins, screened by following experiment:
Adopt the Radix Astragali content assaying method of States Pharmacopoeia specifications, measure the Astragaloside content of medical material, and Radix Astragali total saponins is extracted to the Milkvetch Root of different Ji Yuan, the place of production and the time limit.Consider medical material, Radix Astragali total saponins target product and then determine final raw medicinal material.Detailed results sees the following form.
Comprehensive above-mentioned experimental result, raw medicinal material Ji Yuan elects Radix Astragali as, the place of production: body in Zhangjiakou Area, Hebei Province, Heilungkiang Hulan County, the time limit: life in 1 year, requires that in crude drug, Astragaloside content should be greater than 0.07%.
Embodiment 2
Get Radix Astragali thin slice 1000g (body in Zhangjiakou Area, Hebei Province product Radix Astragali), the 12L that adds water refluxes twice, each 2 hours, merge extracted twice liquid, be condensed into the thick extractum that proportion is 1.25, adding ethanol makes alcohol precipitation concentration be 85%, be stirred to precipitation to separate out completely, filter, supernatant concentration is to clear paste (every 1ml contains medical material amount 0.5g), adjust pH to be 9 with 60%NaOH solution, placement is spent the night.Alkali treatment liquid is directly gone up AB-8 macroporous adsorptive resins and is adsorbed, and with 15L deionized-distilled water eluting saccharide, then decolours with 8L 20% alcoholic solution.Finally with 8L 80% alcoholic solution eluting Radix Astragali saponin, add a small amount of water dissolution after eluent concentrate drying, hold over night, filter and to obtain precipitation.Get and be deposited in 80 DEG C of vacuum dryings, to obtain final product.Adopt HPLC-ELSD (with reference to content measuring standard under version Chinese Pharmacopoeia in 2010 Milkvetch Root item) to measure Astragaloside content, content is 69.6%; Adopt UV to measure Radix Astragali total saponins content, content is 94.7%; It is 0.132% that gravimetric method records yield.
Embodiment 3
Get Radix Astragali thin slice 1000g (body in Zhangjiakou Area, Hebei Province product Radix Astragali), add water to the calorimetric of submergence medical material to reflux three times, each 1 hour, merge three extracting solution, be condensed into the thick extractum of 1/2 of raw medicinal herbs amount, add ethanol and make alcohol precipitation concentration be 80%, be stirred to and precipitate completely, reclaim and filter rear supernatant concentration to clear paste (every 1ml contains medical material amount 0.6g), adjust pH to be 9 with 40%NaOH solution, placement is spent the night.Alkali treatment liquid is directly gone up AB-8 macroporous adsorptive resins and is adsorbed.Alkali treatment liquid is directly gone up AB-8 macroporous adsorptive resins and is adsorbed, and with 10L deionized-distilled water eluting saccharide, then decolours with 5L 20% alcoholic solution.Finally with 6L 80% alcoholic solution eluting Radix Astragali saponin, add a small amount of water dissolution after eluent concentrate drying, hold over night, filter and to obtain precipitation.Get and be deposited in 80 DEG C of vacuum dryings, to obtain final product.Adopting HPLC-ELSD (with reference to content measuring standard under version Chinese Pharmacopoeia in 2010 Milkvetch Root item) to measure Astragaloside content is 68.8%; Adopt UV to measure Radix Astragali total saponins content, content is 94.1%; Gravimetric detemination yield is 0.139%.
Embodiment 4
Get Radix Astragali thin slice 2000g (Heilungkiang Hulan County produces Radix Astragali), the 20L that adds water refluxes twice, each 1.5 hours, merge extracted twice liquid, be condensed into the thick extractum that proportion is 1.30, add ethanol and make alcohol precipitation concentration be 75%, be stirred to and precipitate completely, reclaim and filter rear supernatant concentration to clear paste (every 1ml contains medical material amount 1.0g), adjust pH to be 8 with 60%NaOH solution, placement is spent the night.Alkali treatment liquid is directly gone up AB-8 macroporous adsorptive resins and is adsorbed, and with 20L deionized-distilled water eluting saccharide, then decolours with 8L 30% alcoholic solution.Finally with 10L 95% alcoholic solution eluting Radix Astragali saponin, add a small amount of water dissolution after eluent concentrate drying, hold over night, filter and to obtain precipitation.Get and be deposited in 80 DEG C of vacuum dryings, to obtain final product.Adopting HPLC-ELSD (with reference to content measuring standard under version Chinese Pharmacopoeia in 2010 Milkvetch Root item) to measure Astragaloside content is 70.5%; Adopt UV to measure Radix Astragali total saponins content, content is 95%; Gravimetric detemination yield is 0.264%.
Claims (2)
1. from Chinese medicine astragalus, extract a method for Radix Astragali total saponins, it is characterized in that, comprise the following steps:
A, get Radix Astragali raw medicinal herbs, add water, circumfluence distillation, is concentrated into thick extractum;
B, thick extractum add ethanol makes concentration of alcohol reach 70 ~ 90%, and be stirred to after precipitation separates out completely, filter, supernatant concentration, to clear paste, is 8 ~ 10 by aqueous slkali adjust ph, and hold over night, obtains alkali treatment liquid;
C, get alkali treatment liquid and join macroporous adsorptive resins, with the deionized-distilled water eluting carbohydrate fraction of 10 ~ 15 times of column volumes, again with 20 ~ 30% of 5 ~ 10 times of column volumes ethanol elution, finally with 75 ~ 95% of 5 ~ 10 times of column volumes ethanol elution, collect high concentration ethanol eluent, add a small amount of water dissolution after concentrate drying, leave standstill 12 ~ 48 hours, filter to obtain precipitation;
D, taking precipitate are dried, and are Radix Astragali total saponins.
2. the method for extraction Radix Astragali total saponins according to claim 1, is characterized in that, the aqueous slkali in described step b is the sodium hydroxide solution of mass concentration 30 ~ 60%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093240A (en) * | 2016-06-07 | 2016-11-09 | 山西大学 | A kind of fast-growing Radix Astragali and the discrimination method of the wild Radix Astragali |
| CN106236820A (en) * | 2016-08-26 | 2016-12-21 | 黑龙江珍宝岛药业股份有限公司 | A kind of Radix Astragali injection and preparation method thereof and pharmaceutical composition |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1425674A (en) * | 2002-12-19 | 2003-06-25 | 上海博泰医药科技有限公司 | Process for preparing astraglus base total saponin |
| CN102488742A (en) * | 2011-12-16 | 2012-06-13 | 哈药集团中药二厂 | Preparation method of astragaloside |
| CN104107211A (en) * | 2014-07-29 | 2014-10-22 | 黑龙江珍宝岛药业股份有限公司 | Preparation method of astragalosides extract |
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- 2015-04-13 CN CN201510172731.9A patent/CN104739920A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1425674A (en) * | 2002-12-19 | 2003-06-25 | 上海博泰医药科技有限公司 | Process for preparing astraglus base total saponin |
| CN1282654C (en) * | 2002-12-19 | 2006-11-01 | 上海博泰医药科技有限公司 | Process for preparing astraglus base total saponin |
| CN102488742A (en) * | 2011-12-16 | 2012-06-13 | 哈药集团中药二厂 | Preparation method of astragaloside |
| CN104107211A (en) * | 2014-07-29 | 2014-10-22 | 黑龙江珍宝岛药业股份有限公司 | Preparation method of astragalosides extract |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093240A (en) * | 2016-06-07 | 2016-11-09 | 山西大学 | A kind of fast-growing Radix Astragali and the discrimination method of the wild Radix Astragali |
| CN106236820A (en) * | 2016-08-26 | 2016-12-21 | 黑龙江珍宝岛药业股份有限公司 | A kind of Radix Astragali injection and preparation method thereof and pharmaceutical composition |
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Application publication date: 20150701 |