CN1709916A - Method for extracting high purity polysaccharide of membranous milk vetch and saponin of same - Google Patents
Method for extracting high purity polysaccharide of membranous milk vetch and saponin of same Download PDFInfo
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- CN1709916A CN1709916A CN 200510042836 CN200510042836A CN1709916A CN 1709916 A CN1709916 A CN 1709916A CN 200510042836 CN200510042836 CN 200510042836 CN 200510042836 A CN200510042836 A CN 200510042836A CN 1709916 A CN1709916 A CN 1709916A
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- astragaloside
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Abstract
The invention belongs to the producing method of a kind of high purity radix astragali polysaccharide (RAPS) and astragalus saponin (AS). Its steps are: comminute radix astragali to granulated, after weighed, add six times quantities of mix solvent which is comprised of ethanol, water and n-butanol with proportion of 4 : 3 : 3; send gas into the pot, heat to boil the medicine fluid, circumfluence to distill, filtrate to get distilled liquid A; then add six times of distilled water as per weight proportion into filtrated medicine residue, steam heat to distill, filtrate to get distilled liquid B; mix distilled liquid A and B in liquid tank; then make the mixed A and B distilled liquid have twofold purification of ultra filtering - column chromatogram - solvent recrystallization, and ultra filtering - mellow sedimentation - solvent wash twofold purification method, to respectively get two kinds of products of high purity RAPS and AS. The products have good appearance, in industrial production, the distilling rate of RAPS and AS can respectively get to 94.5% and 92.3%, which are much higher than that of water distilling method and mellow distilling method reported in present literatures.
Description
Technical field
The invention belongs to the production method of high purity astragalus polysaccharides, astragaloside.
Background technology
Have in recent years much and extract astragalus polysaccharides process modification and Study on optimized report: publish pharmaceutical college of Shihezi Univ utilization microwave technology as Chinese materia medica journal .2201.029 (006) .35-36 and extract astragalus polysaccharides with poach alcohol precipitation extraction astragalus polysaccharides method about the poach alcohol precipitation, can make the reaction times shorten about 12 times, polysaccharide content reaches 6.55%; The Li Hongmin of Northwest University etc. are at Northwest University's journal: studies show that of natural science edition .2000.030 (006) .-509-510 record, and adopt the alkali aqueous solution extraction method that the polysaccharide yield is obviously improved, be respectively 11.7% and 5.7%; Chinese materia medica magazine .1998.023 (005) .-284-286 has introduced people such as the graduate Ni Yan of Shanxi Chinese materia medica and has designed orthogonal experiment, optimization to astragalus polysaccharides poach extraction process studies show that, the yield of Radix Astragali Crude polysaccharides, for different extraction times evident difference is arranged, the polysaccharide yield of optimised process is 2.0%, and total polysaccharides content is 37.5% (cryodrying); The Japanese plum treasure of China Academy of TCM waits at herbal medicine .195.026 (008) .-408-410 the sugared content of the different extraction process gained of Radix Astragali Crude polysaccharides is contrasted, wherein utilize the polysaccharide crude extract of ultrafiltration process gained, exceed 20% than poach alcohol deposition method sugar degree, but the Crude polysaccharides yield is lower; The envelope Silans of Lanzhou medical college etc. are at Chinese patent medicine 1997.12.25; 19 (12): 5-6 also carries out orthogonal experiment research to extraction of Astragalus Polysaccharides in Astragalus technology, with astragalus polysaccharides content is judgement criteria, take into account moisture, ash content, reach insolubles index in the water, found that, astragalus polysaccharides content is relevant with alcohol concn, liquor strength and drying means in the technical process, determine soup proportion be 1.05 o'clock be optimised process with 80% ethanol sedimentation, spraying drying.
Research about high purity astragaloside and polysaccharide extracting process has: Chinese patent [application number: 001009690.7; Publication number: 133082; Open day: 2002.01.09; Main classification number: C08B37/00] astragalus polysaccharides of Chinese agricultural university invention and the extraction and separation method of astragaloside disclosed, this invention has been adopted and has been crossed resin column technology or employing ultrafiltration, crossed resin column technology, add in the united extraction sepn process with means such as constituents, to greatest extent polysaccharide in the Radix Astragali and saponin are separated, and can be obtained higher polysaccharide of purity and the smart powder of saponin simultaneously; Chinese patent discloses [application number: 02155002.6; Publication number: 1425674; Open day: 2003.06.25; Main classification number: C07H17/07] patent of invention---the preparation method of Radix Astragali total saponins of the rich safe medical sci-tech in Shanghai company application.This method is to be raw material with the Radix Astragali, more than 2 times, goes up the macroporous adsorbent resin post through the hydro-thermal refluxing extraction behind the extracting liquid filtering, carries out desugar, processed, and separation and purification gets the Radix Astragali total saponins mixture again; The high purity astragalus polysaccharides processing technology of Capital Normal University's exploitation adopts separation means such as film dialysis, and product purity reaches 70-80%[project year numbering: 0100280040].
Summary of the invention
Mainly contain polysaccharide, saponin, flavones, protein, Mierocrystalline cellulose and trace element etc. in the Radix Astragali.Polysaccharide content is about about 20% in the natural Radix Astragali, and astragaloside content is lower, is about about 2%.The extraction of astragalus polysaccharides and astragaloside at present mainly contains water extraction and alcohol extracting method.Astragalus polysaccharides is generally taked water extraction and alcohol precipitation method, and yield and content are lower, and purification refine technology is loaded down with trivial details; Astragaloside has the poach alcohol precipitation to get supernatant liquor and alcohol extracting method, refining employing alcohol extracting, and n-butanol extraction afterwards concentrates finished product then, and solvent load is bigger.For improving the extraction yield and the purity of astragalus polysaccharides, astragaloside, reduce production costs, we have carried out, and high purity astragalus polysaccharides, astragaloside extract, the research of purifying process.
The objective of the invention is to be achieved through the following technical solutions:
The extracting method of a kind of high purity astragalus polysaccharides, astragaloside the steps include:
A), astragalus membranaceus powder is broken to particulate state, after the weighing, add the mixed solvent of 6 times of amounts, mixed solvent is ethanol, water and propyl carbinol, ethanol: water: propyl carbinol=4: 3: 3;
B), steam fed jar in, heat 75-80 ℃, make the soup boiling, the solvent vapo(u)r that produces in the leaching process passes back in the extractor after cooling, extracts 1.8-2.5 hour, filtration obtains extracting solution A;
C), the dregs of a decoction after will filtering, add the distilled water of 6 times of amounts by weight, in steam was fed jar, a temperature was 95-100 ℃ in jar, extracts 1.5-2 hour, filtration obtains extracting solution B;
D), united extraction liquid A, B.
E), with mixed A, B extracting solution, adopt hyperfiltration process, obtain being rich in two kinds of products of astragalus polysaccharides and astragaloside respectively;
F), the ultrafiltrated that will be rich in astragaloside carries out column chromatography, the double purifying of solvent extraction, the high purity astragaloside.
G), will be rich in the astragalus polysaccharides ultrafiltrated and carry out alcohol precipitation, the double purifying of solvent wash, the high purity astragalus polysaccharides.
This invention obtains multinomial technological breakthrough and innovation in process of production, mainly contains following characteristics:
(1) characteristics different with polarity according to the structure of astragalus polysaccharides and astragaloside, we at first adopt mixed solvent (ethanol, water, propyl carbinol) that polysaccharide in the Radix Astragali and saponin are extracted, thin-layer chromatography chromatogram (TLC) analysis revealed, saponin component all extracts in the Radix Astragali.Then residue water is carried, by orthogonal experiment optimization, obtained astragalus polysaccharides and astragaloside optimum extraction production technique, astragalus polysaccharides and astragaloside extraction yield reach 94.5% and 92.3% respectively in the industrial production.
(2) adopt ultra-filtration technique rough segmentation astragalus polysaccharides and astragaloside.Crude extract is ultrafiltration at first, obtains being rich in two kinds of products of astragalus polysaccharides and astragaloside respectively.Equipment adopts the hollow fiber ultrafiltration membrane of the cheapness of domestic scale operation.Ultrafiltration has following advantage than alcohol precipitation and flucculation process commonly used in the Chinese medicine production: 1. the time lacks, and alcohol precipitation and flocculation generally need be left standstill for some time; 2. product loss is few, and alcohol precipitation and flocculation had the astragaloside compounds to separate out in the sedimentary while of macromole, influences product yield; 3. do not influence the chemical constitution and the quality of astragaloside, can reach the production purpose in room temperature with need not to add under other any chemical reagent conditions, flucculation process need add other chemical reagent and alcohol precipitation is with flocculating particularly, has residual flocculation agent like this in product solution.4. hollow fiber ultrafiltration membrane can be regenerated by acid-alkali washing, recycling.
Obtain content respectively greater than 50% astragalus polysaccharides and astragaloside product by hyperfiltration process.
(3) astragaloside makes the finished product saponin content greater than 80% through the double purifying of column chromatography-solvent; To be rich in the astragaloside ultrafiltrated and carry out column chromatography purification, can remove other small molecular weight impurities.By dynamic adsorption and Staticadsorption experiment, we find best column chromatography sorbent material and eluent, and under optimum process condition, the content of astragaloside reaches 83% (ultraviolet spectrometry degree light method).
(4) astragalus polysaccharides makes the finished product polysaccharide content greater than 80% through alcohol precipitation, the double purifying of solvent wash; To be rich in the astragalus polysaccharides ultrafiltrated and carry out alcohol precipitation, can remove other macromole impurity.By solvent wash, product is further purified at last.Make that astragalus polysaccharides content reaches 86% in the product.
(5) adopt respectively lyophilize and moment drying process with atomizing, thereby guarantee astragalus polysaccharides and astragaloside natural product not because of complete processing changes its characteristic, product appearance is preferable simultaneously, it is faint yellow that astragalus polysaccharides is, astragaloside is pale brown look.
(6) same production unit adopts different purification process and step, and astragalus polysaccharides and astragaloside can provide the product of 50%, 70%, 80% 3 specification respectively.
In sum, in the extraction of relevant high purity astragalus polysaccharides and saponin, the application of poach alcohol deposition method, ultra-filtration technique, spray drying technology etc., domestic existing patented technology and bibliographical information.But this problem intends adopting mixed solvent to extract high purity astragalus polysaccharides and saponin, make astragalus polysaccharides and saponin extraction yield reach 94.5% and 92.3% respectively, astragaloside is through the double purifying of column chromatography-solvent recrystallization, astragalus polysaccharides makes the finished product polysaccharide and saponin content respectively greater than 80% through the double purifying of alcohol precipitation-solvent wash, does not domesticly see identical report.
Embodiment
Embodiment 1
Astragalus membranaceus powder is broken to particulate state, claims 1 ton HUANGQI KELI, add 6 tons mixed solvent, mixed solvent is ethanol, water and propyl carbinol, ethanol: water: propyl carbinol=4: 3: 3; Steam is fed in the chuck of extractor, heat 78 ℃, make the soup boiling, the solvent vapo(u)r that produces in the leaching process passes back in the extractor after the cooling of tank top, extracts 2 hours, filters, and extracts extracting solution A out to container for storing liquid with pump; The dregs of a decoction after will filtering again add the distilled water of 6 times of amounts by weight, and in the chuck that steam is fed jar, a temperature is 100 ℃ in jar, extracts 1.8 hours, filter, with pump extraction extracting solution B to container for storing liquid; United extraction liquid A, B are in container for storing liquid; With mixed A, B extracting solution, adopt hyperfiltration process, obtain being rich in two kinds of products of astragalus polysaccharides and astragaloside respectively; The ultrafiltrated that is rich in astragaloside is carried out column chromatography, the double purifying of solvent extraction, get the high purity astragaloside; To be rich in the astragalus polysaccharides ultrafiltrated and carry out alcohol precipitation, the double purifying of solvent wash, get the high purity astragalus polysaccharides.
Embodiment 2
Astragalus membranaceus powder is broken to particulate state, after the weighing, adds the mixed solvent of 6 times of amounts.Mixed solvent is ethanol, water and propyl carbinol, ethanol: water: propyl carbinol=4: 3: 3; Steam is fed in the chuck of extractor, heat 80 ℃ and make the soup boiling, the solvent vapo(u)r that produces in the leaching process passes back in the extractor after the cooling of tank top, extracts 2.2 hours, filters, and extracts extracting solution A out to container for storing liquid with pump; With the dregs of a decoction after filtering, add the distilled water of 6 times of amounts by weight, steam is fed in the chuck of jar, a temperature is 100 ℃ in jar, extracts 1.5 hours, filters, and extracts extracting solution B out to container for storing liquid with pump; United extraction liquid A, B are in container for storing liquid; With mixed A, B extracting solution, adopt hyperfiltration process, obtain being rich in two kinds of products of astragalus polysaccharides and astragaloside respectively; The ultrafiltrated that is rich in astragaloside is carried out column chromatography, the double purifying of solvent extraction, get the high purity astragaloside; To be rich in the astragalus polysaccharides ultrafiltrated and carry out alcohol precipitation, the double purifying of solvent wash, get the high purity astragalus polysaccharides.
Claims (1)
1, the extracting method of a kind of high purity astragalus polysaccharides, astragaloside the steps include:
A), astragalus membranaceus powder is broken to particulate state, after the weighing, add the mixed solvent of 6 times of amounts, mixed solvent is ethanol, water and propyl carbinol, ethanol: water: propyl carbinol=4: 3: 3;
B), steam fed jar in, heat 75-80 ℃, make the soup boiling, the solvent vapo(u)r that produces in the leaching process passes back in the extractor after cooling, extracts 1.8-2.5 hour, filtration obtains extracting solution A;
C), the dregs of a decoction after will filtering, add the distilled water of 6 times of amounts by weight, in steam was fed jar, a temperature was 95-100 ℃ in jar, extracts 1.5-2 hour, filtration obtains extracting solution B;
D), united extraction liquid A, B.
E), with mixed A, B extracting solution, adopt hyperfiltration process, obtain being rich in two kinds of products of astragalus polysaccharides and astragaloside respectively;
F), will be rich in the astragaloside ultrafiltrated and carry out column chromatography, the double purifying of solvent extraction, the high purity astragaloside.
G), will be rich in the astragalus polysaccharides ultrafiltrated and carry out alcohol precipitation, the double purifying of solvent wash, the high purity astragalus polysaccharides.
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| CN 200510042836 CN1709916A (en) | 2005-06-15 | 2005-06-15 | Method for extracting high purity polysaccharide of membranous milk vetch and saponin of same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619107B (en) * | 2009-08-17 | 2011-06-29 | 杭州科皇饲料有限公司 | Astragalus polysaccharide extraction method |
| CN102443072A (en) * | 2010-10-12 | 2012-05-09 | 沈阳药科大学 | Method for simultaneously extracting polysaccharides and saponins from astragalus |
| CN102875688A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Process for extracting polysaccharide from milkvetch roots |
| CN103709261B (en) * | 2013-11-21 | 2016-09-14 | 福建中农牧生物药业有限公司 | A kind of Extraction method for high-content radix astragali polysaccharide |
-
2005
- 2005-06-15 CN CN 200510042836 patent/CN1709916A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619107B (en) * | 2009-08-17 | 2011-06-29 | 杭州科皇饲料有限公司 | Astragalus polysaccharide extraction method |
| CN102443072A (en) * | 2010-10-12 | 2012-05-09 | 沈阳药科大学 | Method for simultaneously extracting polysaccharides and saponins from astragalus |
| CN102875688A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Process for extracting polysaccharide from milkvetch roots |
| CN103709261B (en) * | 2013-11-21 | 2016-09-14 | 福建中农牧生物药业有限公司 | A kind of Extraction method for high-content radix astragali polysaccharide |
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