CN101717427B - Process for extracting astragaloside IV - Google Patents
Process for extracting astragaloside IV Download PDFInfo
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- CN101717427B CN101717427B CN 200910250347 CN200910250347A CN101717427B CN 101717427 B CN101717427 B CN 101717427B CN 200910250347 CN200910250347 CN 200910250347 CN 200910250347 A CN200910250347 A CN 200910250347A CN 101717427 B CN101717427 B CN 101717427B
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- radix astragali
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Abstract
The invention relates to the field of medicament extraction and refining, which is a process for extracting astragaloside IV and solves the problems that the products of the prior art has low yield or needs special devices and technology, is not beneficial to generalization and production and the like. The invention provides a simple, effective, high-yield and new extracting process capable of realizing the industrial large-scale production. The process is operated by the following steps of: cutting raw materials in to pieces or coarse grains, adding enzyme for enzymolysis, and after the enzymolysis, extracting the raw materials by water; extracting and refilling the astragaloside IV. The invention combines the enzymolysis method with a water extraction method and an ethanol extraction method, such that the astragaloside IV in the raw materials can be extracted in maximum; the waste of the raw materials is avoided, the production rate of the astragaloside IV is improved, and the yield of the astragaloside IV is high. In addition, a solution mixing butyl acetate and tert-butyle alcohol is used for refilling, such that the finally obtained product has good quality, stable formation and high yield; and the raw materials are repeatedly and fully utilized in the whole production process, thus the economic efficiency is improved, the environment is protected, and the invention is suitable for the industrial production.
Description
Technical field
The present invention relates to the extract drugs field, is a kind of process for extracting astragaloside IV.
Background technology
The Radix Astragali
Strengthening QI of middle-JIAO is arranged, nourshing blood and promoting blood circulation, inducing diuresis to remove edema, the functions such as strengthening superficial resistance to stop perspiration, mainly contain triterpenoid saponin, flavonoid compound and polysaccharide, take astragalin I (also claiming Cyclosiversioside F) and II as main component, particularly Cyclosiversioside F is commonly used for the leading indicator of quality control in the triterpenoid saponin.The Cyclosiversioside F extracting method mainly contains decocting cooking method, ethanol reflux extraction, ultrasonic extraction, CO
2Supercritical extraction.Ethanol reflux extraction alcohol consumption is very large, and a whole set of refluxing unit need to be arranged.Although the Milkvetch Root quality is comparatively loose, Cyclosiversioside F is water soluble component, the water boiling and extraction Cyclosiversioside F yield lower (usually only less than 0.2%) of existing report, ultrasonic extraction, CO
2Though supercritical extraction can improve the Cyclosiversioside F yield, need special or complicated equipment, that also is that all right is ripe in commercial scale production.Adopt enzymolysis process to there is not yet report in conjunction with the extracting method that extracts Cyclosiversioside F without pure liquid phase extraction process.And present method has also adopted a kind of more efficiently process for purification, and adopt N-BUTYL ACETATE: trimethyl carbinol mixing solutions is made with extra care, and has no report, and by good effect, has improved quality product and purifying efficient.
Summary of the invention
An object of the present invention is as solving above-mentioned prior art products yield lowly or need specific installation and technology, be unfavorable for promoting the problem such as productions, provide a kind of effectively simple, the product yield is high, can realize the new extraction process of mass-producing, industrialization production.This technique operates in accordance with the following steps:
With raw material section or coarse grain, and add enzyme and carry out enzymolysis, use water extraction after the enzymolysis; Extraction; Refining.
Specifically, extraction step is: selected Radix Astragali rhizome section 1kg, add 2-5 times of water, and add enzyme, carry out enzymolysis, leaching process divides 2-4 time, each deionized water extraction 1h-5d with 6-14 times of Radix Astragali quality; After water extraction liquid was concentrated with filter paper filtering, the concentration that adds 2-4 times of concentrated solution volume surpassed 90% ethanol, leaves standstill more than the 16h, filtered and removed precipitation, concentrated Radix Astragali total saponins concentrated solution, the Recycled ethanol of obtaining of filtrate;
Extraction: use concentrated solution volume 1/4-1 petroleum ether extraction degreasing doubly more than 2 times the Radix Astragali total saponins concentrated solution that obtains, each extraction 2-4h, merge lower floor's solution, water-saturated n-butanol with 1/4-1 times of degreasing concentrated solution volume repeats to extract 2-4 time again, more than each extraction 1h, merge n-butanol layer, rotary evaporation, the dry Radix Astragali total saponins crude product that gets;
Refining: the Radix Astragali total saponins crude product adds 4-6 times of N-BUTYL ACETATE: the solution of the trimethyl carbinol (1: 1), stir, and to filter after placing, drying precipitate namely gets the finished product, and filtrate is reclaimed.
Furtherly:
Selected Radix Astragali rhizome section adds 3 times of water, adds enzyme, carries out enzymolysis, and leaching process divides 2 times, the deionized water extraction 24h of 12 times of Radix Astragali quality of the 1st usefulness; The 2nd amount of water is 10 times of Radix Astragali quality, extracts 20h.After water extraction liquid is concentrated into small volume with filter paper filtering, add 95% ethanol of 3 times of concentrated solution volumes, leave standstill 24h, filter and remove precipitation, filtrate is concentrated, Recycled ethanol.
Extraction: with the Radix Astragali total saponins concentrated solution that obtains with the petroleum ether extraction degreasing of 1/3 volume 3 times, each extraction 3h, merge lower floor's solution, use again the water-saturated n-butanol re-extract 3 times of 1/3 degreasing concentrated solution volume, each extraction 2h, merge n-butanol layer, rotary evaporation, the dry Radix Astragali total saponins crude product that gets.
Refining: the Radix Astragali total saponins crude product adds 5 times of N-BUTYL ACETATEs: the solution of the trimethyl carbinol (1: 1), stir, and to filter after placing, drying precipitate namely gets the finished product, and filtrate is reclaimed.
The enzyme that adds in the described extraction step is to add with the form of enzymolysis solution, and the consumption of described enzymolysis solution is the 0.5-5% of raw materials quality, and hydrolysis temperature is 30-50 ℃, and enzymolysis time is 2-5 hour.
Wherein said enzymolysis solution can be cellulase.Can also be the prozyme of cellulase and distiller's yeast enzyme, in the quality percentage composition, cellulase be 40-100%, and the distiller's yeast enzyme is 0-60%; Preferably, cellulase is 50-80%, and the distiller's yeast enzyme is 20-50%; More preferably cellulase is 60%, and the distiller's yeast enzyme is 40%.Can also comprise amylase in the described enzymolysis solution, in the quality percentage composition, cellulase is 40-100%, and the distiller's yeast enzyme is 0-60%, and amylase is 0-40%.The preferred cellulose enzyme is 50-60%, and the distiller's yeast enzyme is 20-40%, amylase be 10-20%. most preferably cellulase be 50%, the distiller's yeast enzyme is 35%, amylase is 15%.
The concentration of described enzymolysis solution is 2%-10%.Can add with the enzymolysis solution form of working good in the raw material, also can mix respectively the mixture that forms raw material and enzymolysis solution with raw material with the form of aqueous solvent and enzyme.
Beneficial effect of the present invention is:
The present invention unites the way method that enzymolysis process and water extraction alcohol extracting combine, so that the Cyclosiversioside F in the raw material is extracted dramatically, avoided to the utmost the waste of raw material, improved the productivity of Cyclosiversioside F, yield has improved more than 80%, output is high, and the good product quality that makes, and it is stable to be shaped.And whole production process has been accomplished repeatedly taking full advantage of of raw material, has not only improved economic benefit, has accomplished especially utilization of waste material, protection of the environment, and whole process is fit to suitability for industrialized production.
Treating process of the present invention has changed the sodium hydroxide solution alkali wash of in the past commonly using, and adopts N-BUTYL ACETATE: the trimethyl carbinol is refining, and process is simple, and solvent can reclaim, and pollutes little, effective.
Embodiment
Embodiment 1
Selected Radix Astragali rhizome section 1kg adds 2 times of water, adds enzyme, carries out enzymolysis, and leaching process divides 2 times, the deionized water extraction 4d of 12 times of Radix Astragali quality of the 1st usefulness; The 2nd amount of water is 10 times of Radix Astragali quality, extracts 3d.Water extraction liquid is also concentrated with filter paper filtering, adds 95% ethanol of 3 times of concentrated solution volumes, leaves standstill 24h, filters to remove and precipitates, and filtrate is concentrated, Recycled ethanol.
Extraction: with the Radix Astragali total saponins concentrated solution that obtains with the petroleum ether extraction degreasing of 1/3 volume 3 times, each extraction 3h, merge lower floor's solution, use again the water-saturated n-butanol re-extract 3 times of 1/3 degreasing concentrated solution volume, each extraction 2h, merge n-butanol layer, rotary evaporation, the dry Radix Astragali total saponins crude product that gets.
Refining: the Radix Astragali total saponins crude product adds 5 times of N-BUTYL ACETATEs: the solution of the trimethyl carbinol (1: 1), stir, and to filter after placing, drying precipitate namely gets the finished product, and filtrate is reclaimed.
The enzyme that adds in the described extraction step is to add with the form of enzymolysis solution, and the consumption of described enzymolysis solution is the 0.5-5% of raw materials quality, and hydrolysis temperature is 30-50 ℃, and enzymolysis time is 2-5 hour.
The enzyme cellulase of wherein said enzymolysis solution is 60%, and the distiller's yeast enzyme is 40%.
Embodiment 2
Selected Radix Astragali rhizome section 1kg adds 5 times of water, adds enzyme, carries out enzymolysis, and leaching process divides 3 times, the deionized water extraction 4d of 8 times of Radix Astragali quality of the 1st usefulness; The 2nd amount of water is 7 times of Radix Astragali quality, extracts 3d, uses for the third time 6 times of water extraction 4h.Water extraction liquid is also concentrated with filter paper filtering, adds 98% ethanol of 2 times of concentrated solution volumes, leaves standstill 20h, filters to remove and precipitates, and filtrate is concentrated, Recycled ethanol.
Extraction: with the Radix Astragali total saponins concentrated solution that obtains with the petroleum ether extraction degreasing of 1/2 volume 3 times, each extraction 3h, merge lower floor's solution, use again the water-saturated n-butanol re-extract 3 times of 1/2 degreasing concentrated solution volume, each extraction 2h, merge n-butanol layer, rotary evaporation, the dry Radix Astragali total saponins crude product that gets.
Refining: the Radix Astragali total saponins crude product adds 4 times of N-BUTYL ACETATEs: the solution of the trimethyl carbinol (1: 1), stir, and to filter after placing, drying precipitate namely gets the finished product, and filtrate is reclaimed.
The enzyme that adds in the described extraction step is to add with the form of enzymolysis solution, and the consumption of described enzymolysis solution is raw materials quality 2%, and hydrolysis temperature is 40 ℃, and enzymolysis time is 3 hours.
Embodiment 3-11
In the 10kg raw material, the consumption of enzyme and composition, and enzymolysis time and temperature are as shown in the table, all the other are with embodiment 1:
| Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 | |
| Enzyme dosage (kg) | 0.2 | 0.1 | 0.3 | 0.15 | 0.25 | 0.18 | 0.22 | 0.27 | 0.12 |
| Hydrolysis temperature (℃) | 30 | 50 | 40 | 35 | 45 | 38 | 42 | 48 | 33 |
| Enzymolysis time (h) | 3 | 3.2 | 3.5 | 5 | 3.8 | 4 | 4.2 | 4.5 | 1 |
| Cellulase content (%) | 100 | 40 | 50 | 60 | 50 | 70 | 55 | 80 | 90 |
| Distiller's yeast enzyme content (%) | 0 | 60 | 40 | 20 | 35 | 25 | 5 | 20 | 0 |
| Amylase content (%) | 0 | 0 | 10 | 20 | 15 | 5 | 40 | 0 | 10 |
Claims (3)
1. a process for extracting astragaloside IV is characterized in that, this technique operates in accordance with the following steps:
Raw material is cut into slices;
Enzymolysis and extraction: selected Radix Astragali rhizome section 1kg, add 2-5 times of water, add enzyme, carry out enzymolysis; Leaching process divides 2-4 time, each deionized water extraction 1h-5d with 6-14 times of Radix Astragali quality; After water extraction liquid was concentrated with filter paper filtering, the concentration that adds 2-4 times of concentrated solution volume surpassed 90% ethanol, leaves standstill more than the 16h, filtered and removed precipitation, concentrated Radix Astragali total saponins concentrated solution, the Recycled ethanol of obtaining of filtrate;
Extraction: use concentrated solution volume 1/4-1 petroleum ether extraction degreasing doubly more than 2 times the Radix Astragali total saponins concentrated solution that obtains, each extraction 2-4h, merge lower floor's solution, water-saturated n-butanol with 1/4-1 times of degreasing concentrated solution volume repeats to extract 2-4 time again, more than each extraction 1h, merge n-butanol layer, rotary evaporation, the dry Radix Astragali total saponins crude product that gets;
Refining: the Radix Astragali total saponins crude product adds 4-6 times of N-BUTYL ACETATE: the trimethyl carbinol stirs with the solution of ratio mixing in 1: 1, filters after placing, and drying precipitate namely gets the finished product, the filtrate recovery;
Described enzyme is to add with the form of enzymolysis solution, and the consumption of enzymolysis solution is the 0.5-5% of raw materials quality, and hydrolysis temperature is 30-50 ℃, and enzymolysis time is 2-5 hour;
Described enzymolysis solution cellulase is 50-60%, and the distiller's yeast enzyme is 20-40%, and amylase is 10-20%.
2. process for extracting astragaloside IV according to claim 1 is characterized in that, extraction step is: selected Radix Astragali rhizome section, add 3 times of water, and add enzyme, carry out enzymolysis, leaching process divides 2 times, the deionized water extraction 24h of 12 times of Radix Astragali quality of the 1st usefulness; The 2nd amount of water is 10 times of Radix Astragali quality, extracts 20h; Water extraction liquid is also concentrated with filter paper filtering, adds 95% ethanol of 3 times of concentrated solution volumes, leaves standstill 24h, filters to remove and precipitates, and filtrate is concentrated, Recycled ethanol;
Extraction: with the Radix Astragali total saponins concentrated solution that obtains with the petroleum ether extraction degreasing of 1/3 volume 3 times, each extraction 3h, merge lower floor's solution, use again the water-saturated n-butanol re-extract 3 times of 1/3 degreasing concentrated solution volume, each extraction 2h, merge n-butanol layer, rotary evaporation, the dry Radix Astragali total saponins crude product that gets;
Refining: the Radix Astragali total saponins crude product adds 5 times of N-BUTYL ACETATEs: the trimethyl carbinol stirs with the solution of ratio mixing in 1: 1, filters after placing, and drying precipitate namely gets the finished product, the filtrate recovery.
3. process for extracting astragaloside IV according to claim 1 is characterized in that, described enzymolysis solution cellulase is 50%, and the distiller's yeast enzyme is 35%, and amylase is 15%.
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| CN 200910250347 CN101717427B (en) | 2009-12-04 | 2009-12-04 | Process for extracting astragaloside IV |
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| CN 200910250347 CN101717427B (en) | 2009-12-04 | 2009-12-04 | Process for extracting astragaloside IV |
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| CN101717427A CN101717427A (en) | 2010-06-02 |
| CN101717427B true CN101717427B (en) | 2013-02-27 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109125381A (en) * | 2018-09-05 | 2019-01-04 | 湖南中茂生物科技有限公司 | A method of promoting astragalus root total saponin conversion |
| CN109105899B (en) * | 2018-09-10 | 2022-11-29 | 齐鲁工业大学 | Method for preparing high-activity IBD medical food raw material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569884A (en) * | 2004-04-29 | 2005-01-26 | 南京医科大学 | Method for preparing astragaloside and its use in preparation of drug for preventing and treating diabetic nephropathy |
| CN101130802A (en) * | 2007-07-30 | 2008-02-27 | 金凤燮 | Method for preparing astragaloside iv by enzymic hydrolysis for astragalus saponin glycosyl |
| CN101695520A (en) * | 2008-12-30 | 2010-04-21 | 天津医科大学 | Preparation method of medicament for treating diabetes |
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2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569884A (en) * | 2004-04-29 | 2005-01-26 | 南京医科大学 | Method for preparing astragaloside and its use in preparation of drug for preventing and treating diabetic nephropathy |
| CN101130802A (en) * | 2007-07-30 | 2008-02-27 | 金凤燮 | Method for preparing astragaloside iv by enzymic hydrolysis for astragalus saponin glycosyl |
| CN101695520A (en) * | 2008-12-30 | 2010-04-21 | 天津医科大学 | Preparation method of medicament for treating diabetes |
Non-Patent Citations (4)
| Title |
|---|
| 肖丽丽等.黄芪皂苷生物转化物质的分离提取.《大连轻工业学院学报》.2006,第25卷(第2期),86-88. * |
| 蒲军等.漆酶提取黄芪中黄芪皂苷的研究.《中草药》.2005,第36卷(第12期),1809-1811. * |
| 许平平等.酶转化法提高黄芪甲苷的得率.《大连工业大学学报》.2009,第28卷(第1期),20-22. * |
| 郑立颖等.纤维素酶在黄芪有效成分提取中的应用.《甘肃农业大学学报》.2005,第40卷(第1期),94-96. * |
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