CN1880342A - Process for extracting polysaccharide from astragalus root using microwave - Google Patents
Process for extracting polysaccharide from astragalus root using microwave Download PDFInfo
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- CN1880342A CN1880342A CN 200510026889 CN200510026889A CN1880342A CN 1880342 A CN1880342 A CN 1880342A CN 200510026889 CN200510026889 CN 200510026889 CN 200510026889 A CN200510026889 A CN 200510026889A CN 1880342 A CN1880342 A CN 1880342A
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Abstract
This invention discloses a method for extracting Radix Astragali polysaccharide by microwave from Radix Astragali, comprising: 1) extract the Radix Astragali in water using microwave at constant temperature of 40-100Deg C; 2) collect the extracting liquid, filtrate, concentrate and precipitate by adding ethanol; 3) centrifuge and dry the sediment so as to obtain the Radix Astragali polysaccharide. This invention can control the microwave extraction at certain constant temperature continuously without break between each extraction, and is characterized of high selectivity, simple procedures, low consumption of labor and energy, high yield, and high purity.
Description
Technical field
The present invention relates to a kind of Chinese medicine microwave extract method, particularly be meant the method that adopts microwave technology from the Radix Astragali, to extract astragalus polysaccharides.
Background technology
The Radix Astragali (Radix Astragalus) is the dry root of leguminous plants Radix Astragali (Astragalus membranaceus (Fisch) Bge) or Radix Astagali (Astragalus membranaceus (Fisch) Bge.Var.mongholicus (Bge) Hsiao), be important beneficial gas Chinese medicine, it is sweet to distinguish the flavor of, slightly warm in nature, invigorating QI to consolidate the body surface resistance, Li Shui holds in the palm sore.Modern age, pharmacological research showed, astragalus polysaccharides is one of main component of the Radix Astragali, had enhance immunity power, antitumor, Antiradiation injury, antibacterial and anti-viral, blood sugar regulation, the anti-ageing pharmacological action widely of waiting for a long time.
And the Chinese medicine microwave extract method is because of the discharging of no toxic pollutant in its process; In addition, microwave equipment is a consumer, need not be equipped with boiler, safety non-pollution, and belong to green engineering.But adopt the document of microwave method extraction separation astragalus polysaccharides from the Radix Astragali few, as Wang Li, Liu Zhiyong, Shandong Kien Giang etc. (microwave extraction of astragalus polysaccharides and assay [J]. the Chinese materia medica journal, 2001,29 (6): 35.) the utilization microwave technology is with Radix Astragali sherwood oil, ether weeding of grease solubility impurity, remove contained monose with 80% extraction using alcohol, behind interference such as oligose and the glycoside composition, putting into MCL-3 type continuous microwave reactor again continues to adjust power 630W, 600W with water refluxing extraction 20min, 560W, 450W is evaporated to half volume, adds 0.1% activated carbon decolorizing, filter, filtrate adds 95% ethanolic soln to be made and contains alcohol 80%, and standing over night is filtered, the residue ether, the dehydrated alcohol repetitive scrubbing, oven dry promptly gets the astragalus polysaccharides crude product, and content is 6.55%.
Gong Shengzhao, Yang Zhuoru (microwave-assisted extracts the technical study [J] of astragalus polysaccharides. South China Science ﹠ Engineering University's journal (natural science edition), 2004,32 (8): 93-96) with water be extraction agent, studied the technology of microwave-assisted extraction astragalus polysaccharides, obtained the optimum process condition of microwave-assisted extraction astragalus polysaccharides: liquid material mass ratio is 12: 1; Regulating best pH with saturated limewater is 9; Extract 2 times during microwave power 300W; Opened microwave 1 minute during each the extraction, intermittently 1 minute, opened again 1 minute, totally 10 times so repeatedly, promptly extract total time is 19 minutes at every turn, the wherein real microwave extraction time is 10 minutes.Behind the extracting solution vacuum concentration, add ethanol and make polysaccharide precipitation, filter, precipitation with washing with alcohol repeatedly promptly gets Radix Astragali Crude polysaccharides after the vacuum-drying, and productive rate is 14.6%, and purity is 88.1%.
As seen, above-mentioned existing microwave extract method exists: will remove impurity earlier before 1. extracting; 2. extracting power needs always 〉=300W, and continuous open and close microwave reactor repeatedly.Therefore cause operation steps too much, problem such as too numerous and diverse and waste energy.
Summary of the invention
Too much at the operation steps that exists in the aforesaid method, the excessive problem that causes energy dissipation of too numerous and diverse and power, we are to its improvement of having carried out extracting method, make the microwave extraction step simplify and don't cause the waste of the energy, and the astragalus polysaccharides content of gained or extraction yield are all higher.So the purpose of this invention is to provide a kind of method of new extracting polysaccharide from astragalus root using microwave.
Technical scheme of the present invention is: a kind of from the Radix Astragali method of extracting polysaccharide from astragalus root using microwave, it comprises the following steps:
1) Milkvetch Root is carried out the constant temperature microwave extraction in water, this temperature is selected from 40～100 ℃;
2) collect extracting solution, filter, concentrate, add ethanol and obtain precipitation;
3) the precipitation centrifugal drying of this being obtained promptly makes astragalus polysaccharides of the present invention.
When the said constant temperature microwave extraction of the present invention is meant each extraction, directly controlled microwave extract equipment temperature of reaction at certain a bit, extract continuously by the Microwave Extraction Equipment automatic power adjustment, need not constantly artificially to adjust microwave power or carry out extraction at intermittence.As seen as long as can controlled temperature and regulate any microwave reaction device of power automatically or carry (collection) taking equipment and all can be used for the present invention, as: WF-4000C (gerotor type microwave reaction system, Shanghai EU Analytical Instrument Co., Ltd.); WF-4000M (closed microwave reaction system, Shanghai EU Analytical Instrument Co., Ltd.) MAS-I type (the normal pressure microwave-assisted synthesizes/the extractive reaction instrument, Xinyi Microwave Chemistry Tech Co., Ltd.); MDS-6 type (non-pulse formula temperature, pressure dual controlled microwave are cleared up/abstraction instrument Xinyi Microwave Chemistry Tech Co., Ltd.); MDS-2002AT (temperature, pressure dual controlled microwave are cleared up/abstraction instrument Xinyi Microwave Chemistry Tech Co., Ltd.) etc.The present invention chooses WTS03-1 type Microwave Extraction Equipment, when certain some temperature of above-mentioned scope is extracted, removes the of short duration initial period that reaches this temperature, extracts the stage in remainder, and this plant capacity is all below 200W.
Wherein, said extraction time is 1～10 time in the step 1), each 5～30 minutes, adds the water of 5～25 times of weight at every turn.
Preferably, said temperature of the present invention is selected from 60～90 ℃, and microwave extraction 2～6 times each 8～20 minutes, adds 6～15 times of amounts of water at every turn.
More preferably, this temperature is 68～72 ℃, microwave extraction 3～4 times, and each 10 minutes, add 11 times of water gagings first, add 8 times of amounts of water later at every turn.
Preferably, said water can also contain acid or alkali in the step 1) of the present invention, and its pH regulator is 4～8.Preferred mineral acid of said acid or alkali or alkali, example hydrochloric acid, sulfuric acid, potassium hydroxide, sodium hydroxide or ammoniacal liquor etc.Usually select for use 0.5～10% diluted acid or 0.5～5% diluted alkaline to get final product.
The inventive method step 2) with 3) can select for use any present astragalus polysaccharides to separate and the ordinary method and the step of purifying, preferably, step 2) in the said ethanol that adds obtain precipitation (abbreviation alcohol precipitation) and can carry out more than 2 times or 2 times repeatedly.
Milkvetch Root of the present invention can be selected various proterties such as its sheet, piece and powder for use, preferred Milkvetch Root powder.
Compared with prior art, the present invention has the following advantages: step is simple, need not constantly artificial adjustment microwave power or carries out the extraction at intermittence, reduces the manpower consumption; Microwave power of the present invention is held in below the 200W at most of time dimensions, has reduced energy consumption; In addition, the used ethanol of alcohol precipitation is recyclable uses repeatedly; So the inventive method can reduce cost greatly.In addition, the present invention is simple to operate, does not need post, and microwave extraction can shorten extraction time greatly to 20min.And the extraction yield height of the inventive method: generally can be greater than 14%; And the abstraction reaction condition is controlled, and promptly selectivity is good, thereby can prepare the product of high purity (all above 50%, the tallest and the biggest in 87%) repeatedly.
Embodiment
Further specify the present invention below by embodiment.It should be understood that embodiments of the invention are to be used to illustrate the present invention rather than limitation of the present invention.Essence according to the present invention all belongs to the scope of protection of present invention to the simple modifications that the present invention carries out.In addition, in the present invention, (w/w) expression weight percent concentration or weight ratio.
Wherein, the Milkvetch Root of choosing in the following example produces for the Huiyuan, Shanxi, crosses 20 orders; Microwave Extraction Equipment is WTS03-1 type (the outstanding full microwave equipment company limited in Nanjing).Gained astragalus polysaccharides purity adopts the phenolsulfuric acid method to record.
Embodiment 1
Precision takes by weighing Milkvetch Root 10g, puts in the Microwave Extraction Equipment, adds water 114ml for the first time, adds water 80ml later at every turn, and 70 ℃ of controlled temperature extract 4 times altogether, each 10min.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 10ml, add ethanol 50ml and stir, centrifugal, precipitation adds water 150ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 10ml, adding ethanol 50ml stirs, centrifugal, dry purity is 87.14% astragalus polysaccharides 1.4 grams, and productive rate is 14%.
Embodiment 2
Precision takes by weighing Milkvetch Root 5g, puts in the Microwave Extraction Equipment, for the first time adds dilute hydrochloric acid solution 50ml, adds dilute hydrochloric acid solution 25ml later at every turn, and control pH is 4, and 40 ℃ of controlled temperature, extracts each 5min altogether 8 times.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 10ml, add ethanol 50ml and stir, centrifugal, precipitation adds water 150ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 10ml, adding ethanol 50ml stirs, centrifugal, dry purity is 60.23% astragalus polysaccharides 1.02 grams, and productive rate is 20.4%.
Embodiment 3
Precision takes by weighing Milkvetch Root 20g, puts in the Microwave Extraction Equipment, adds ammonia soln 500ml, and control pH is 8, and 100 ℃ of controlled temperature, extracts 1 time 30min.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 13ml, add ethanol 40ml and stir, centrifugal, precipitation adds water 240ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 13ml, adding ethanol 40ml stirs, centrifugal, dry purity is 75.56% astragalus polysaccharides 3.17 grams, and productive rate is 15.85%.
Embodiment 4
Precision takes by weighing Milkvetch Root 15g, puts in the Microwave Extraction Equipment, for the first time adds dilution heat of sulfuric acid 225ml, adds dilution heat of sulfuric acid 200ml later at every turn, and control pH is 5, and 60 ℃ of controlled temperature, extracts each 8min altogether 6 times.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 13ml, add ethanol 55ml and stir, centrifugal, precipitation adds water 230ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 13ml, adding ethanol 55ml stirs, centrifugal, dry purity is 64.78% astragalus polysaccharides 2.46 grams, and productive rate is 16.4%.
Embodiment 5
Precision takes by weighing Milkvetch Root 10g, puts in the Microwave Extraction Equipment, for the first time adds dilute sodium hydroxide aqueous solution 120ml, later repeated hydrogenation aqueous solution of sodium oxide 80ml, and control pH is 8, and 90 ℃ of controlled temperature, extracts each 20min altogether 2 times.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 10ml, add ethanol 50ml and stir, centrifugal, precipitation adds water 150ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 10ml, adding ethanol 50ml stirs, centrifugal, dry purity is 80.12% astragalus polysaccharides 1.48 grams, and productive rate is 14.8%.
Embodiment 6
Precision takes by weighing Milkvetch Root 10g, puts in the Microwave Extraction Equipment, and hydro-oxidation aqueous solutions of potassium 120ml for the first time, later on each hydro-oxidation aqueous solutions of potassium 80ml, control pH is 8, and 60 ℃ of controlled temperature, extracts each 10min altogether 3 times.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 10ml, add ethanol 50ml and stir, centrifugal, precipitation adds water 150ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 10ml, adding ethanol 50ml stirs, centrifugal, dry purity is 67.84% astragalus polysaccharides 1.56 grams, and productive rate is 15.6%.
Embodiment 7
Precision takes by weighing Milkvetch Root 10g, puts in the Microwave Extraction Equipment, adds water 120ml for the first time, adds water 80ml for the second time, and 60 ℃ of controlled temperature extract 3 times altogether, each 10min.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 10ml, add ethanol 50ml and stir, centrifugal, precipitation adds water 150ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 10ml, adding ethanol 50ml stirs, centrifugal, dry purity is 66.78% astragalus polysaccharides 1.53 grams, and productive rate is 15.29%.
Embodiment 8
Precision takes by weighing Milkvetch Root 10g, puts in the Microwave Extraction Equipment, adds water 120ml for the first time, adds water 80ml for the second time, and 70 ℃ of controlled temperature extract 2 times altogether, each 20min.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 10ml, add ethanol 50ml and stir, centrifugal, precipitation adds water 150ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 10ml, adding ethanol 50ml stirs, centrifugal, dry purity is 78.74% astragalus polysaccharides 1.286 grams, and productive rate is 12.86%.
Embodiment 9
Precision takes by weighing Milkvetch Root 10g, puts in the Microwave Extraction Equipment, adds water 120ml for the first time, adds water 80ml for the second time, and 50 ℃ of controlled temperature extract 3 times altogether, each 20min.Collect extracting solution, filter, collect filtrate with gauze and absorbent cotton, be concentrated into 10ml, add ethanol 50ml and stir, centrifugal, precipitation adds water 150ml, stirring makes it dissolving, and is centrifugal, gets supernatant concentration to 10ml, adding ethanol 50ml stirs, centrifugal, dry purity is 66.54% astragalus polysaccharides 0.925 gram, and productive rate is 9.25%.
Claims (10)
1, a kind of from the Radix Astragali method of extracting polysaccharide from astragalus root using microwave, it comprises the following steps:
1) Milkvetch Root is carried out the constant temperature microwave extraction in water, this temperature is selected from 40～100 ℃;
2) collect extracting solution, filter, concentrate, add ethanol and obtain precipitation;
3) the precipitation centrifugal drying of this being obtained promptly makes astragalus polysaccharides of the present invention.
2, the method for claim 1 is characterized in that said extraction time is 1～10 time in the step 1), each 5～30 minutes, adds the water of 5～25 times of weight at every turn.
3, method as claimed in claim 2 is characterized in that this temperature is selected from 60～90 ℃ in the step 1), and microwave extraction 2～6 times each 8～20 minutes, adds 6～15 times of amounts of water at every turn.
4, method as claimed in claim 3 is characterized in that this temperature is 68～72 ℃, microwave extraction 3～4 times, and each 10 minutes, add 11 times of water gagings first, add 8 times of amounts of water later at every turn.
5, the method for claim 1 is characterized in that said water also contains acid or alkali in the step 1), and its pH is 4～8.
6, method as claimed in claim 5 is characterized in that this acid or alkali are mineral acid or alkali.
7, method as claimed in claim 6 is characterized in that this mineral acid is hydrochloric acid or sulfuric acid.
8, method as claimed in claim 6 is characterized in that this mineral alkali is potassium hydroxide, sodium hydroxide or ammoniacal liquor.
9, the method for claim 1 is characterized in that step 2) in the said ethanol that adds obtain precipitation and can carry out more than 2 times or 2 times repeatedly.
10,, it is characterized in that this Milkvetch Root is its powder as each described method of claim 1～9.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100480276C (en) * | 2007-03-29 | 2009-04-22 | 山东大学 | Process of preparing high purity astragalus polysaccharide |
| CN100502887C (en) * | 2007-03-29 | 2009-06-24 | 山东大学 | Buccal tablet of Asraguluspolysacharin |
| CN101240036B (en) * | 2008-02-26 | 2010-06-09 | 西北师范大学 | Microwave auxiliary extraction method for artemisia seed polysaccharide |
| CN102936293A (en) * | 2012-11-28 | 2013-02-20 | 天津科百生物科技研发有限公司 | Extracting and purifying method of fucoidan from fucus vesiculosus |
| WO2013067897A1 (en) * | 2011-11-07 | 2013-05-16 | 沈阳科思高科技有限公司 | Method for extracting polysaccharides from higher plants and fungi through microwave chemical treatment |
| CN101376904B (en) * | 2007-08-29 | 2013-06-19 | 上海医药工业研究院 | Intra-polysaccharides from mycelia of ganoderma sinensis, and preparation and use thereof |
| CN105440147A (en) * | 2015-12-14 | 2016-03-30 | 陈燕妮 | Process for producing astragalus polysaccharide by using microwave technology |
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2005
- 2005-06-17 CN CN 200510026889 patent/CN1880342A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100480276C (en) * | 2007-03-29 | 2009-04-22 | 山东大学 | Process of preparing high purity astragalus polysaccharide |
| CN100502887C (en) * | 2007-03-29 | 2009-06-24 | 山东大学 | Buccal tablet of Asraguluspolysacharin |
| CN101376904B (en) * | 2007-08-29 | 2013-06-19 | 上海医药工业研究院 | Intra-polysaccharides from mycelia of ganoderma sinensis, and preparation and use thereof |
| CN101240036B (en) * | 2008-02-26 | 2010-06-09 | 西北师范大学 | Microwave auxiliary extraction method for artemisia seed polysaccharide |
| US8110677B2 (en) | 2008-02-26 | 2012-02-07 | Northwest Normal University | Microwave-assisted extraction of polysaccharide from Artemisia sphaerocephala |
| WO2013067897A1 (en) * | 2011-11-07 | 2013-05-16 | 沈阳科思高科技有限公司 | Method for extracting polysaccharides from higher plants and fungi through microwave chemical treatment |
| JP2014532788A (en) * | 2011-11-07 | 2014-12-08 | シェンヤン ケシ ハイ−テクノロジー カンパニー リミテッドＳｈｅｎｙａｎｇ Ｋｅｓｉ Ｈｉｇｈ−Ｔｅｃｈｎｏｌｏｇｙ Ｃｏ．Ｌｔｄ | Polysaccharide extraction method of higher plants and fungi based on microwave chemical treatment |
| EP2778177A4 (en) * | 2011-11-07 | 2015-07-29 | Shenyang Kesi High Technology Co Ltd | Method for extracting polysaccharides from higher plants and fungi through microwave chemical treatment |
| US9447198B2 (en) | 2011-11-07 | 2016-09-20 | Shenyang Kesi High-Technology Co. Ltd. | Method for extracting polysaccharides from higher plants and fungi through microwave chemical treatment |
| CN102936293A (en) * | 2012-11-28 | 2013-02-20 | 天津科百生物科技研发有限公司 | Extracting and purifying method of fucoidan from fucus vesiculosus |
| CN102936293B (en) * | 2012-11-28 | 2016-01-20 | 天津科百生物科技研发有限公司 | A kind of extracting and purifying method of fucoidan |
| CN105440147A (en) * | 2015-12-14 | 2016-03-30 | 陈燕妮 | Process for producing astragalus polysaccharide by using microwave technology |
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