CN101550197A - Method for recovering Ginseng polysaccharide form red ginseng alcohol extraction waste material - Google Patents

Method for recovering Ginseng polysaccharide form red ginseng alcohol extraction waste material Download PDF

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CN101550197A
CN101550197A CNA2009100982447A CN200910098244A CN101550197A CN 101550197 A CN101550197 A CN 101550197A CN A2009100982447 A CNA2009100982447 A CN A2009100982447A CN 200910098244 A CN200910098244 A CN 200910098244A CN 101550197 A CN101550197 A CN 101550197A
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panaxan
polysaccharide
red ginseng
ginseng
alcohol extraction
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CN101550197B (en
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刘雪松
王龙虎
马珠凤
陈勇
王治
陈杨胜
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention provides a method for recovering Ginseng polysaccharide form red ginseng alcohol extraction waste material. The extract obtained by alcohol extraction mainly contains the active components such as saponins; and Ginseng polysaccharide can be extracted from the alcohol extraction waste by water extraction process. The invention comprises the processes of: water extracting red ginseng waste residue after alcohol extraction, concentrating, alcohol precipitating, removing protein, drying in vacuum, determining contents and obtaining Ginseng polysaccharide crude product; in which, the polysaccharide content in the crude product is 45-65%, and the polysaccharide yield rate is above 10%. The invention can obtain two effective positions from one medicinal material, thereby increases medicinal material comprehensive utilization rate, fully utilizes waste residue, saves precious Ginseng resource. and the method in the invention is reasonably designed and practical.

Description

A kind of method that from the red ginseng alcohol extraction waste material, reclaims the panaxan
Technical field
The invention belongs to Chinese material medicine resource comprehensive utilization field, relate to a kind of secondary resource exploitation and Chinese medicine composite extracting method of genseng waste, relate in particular to a kind of method that from the red ginseng alcohol extraction waste material, reclaims the panaxan.
Background technology
Red ginseng is the dry root of Araliaceae genseng Panax ginseng after steaming.As famous and precious traditional tonic Chinese medicine material, it has reinforces vital energy, and multiple arteries and veins takes off admittedly, reinforces the spleen to benefit the lung, effect such as promote the production of body fluid, calm the nerves.Red ginseng is usually used in body void and desires to take off clinically, the cold weak pulse of limb, and insufficiency of the spleen food is few, and the deficiency syndrome of the lung is breathed with cough, and Tianjin wound is thirsty, and interior heat is quenched one's thirst, and prolonged illness is empty wins, the palpitation with fear insomnia, the impotence palace is cold; Heart failure, cardiogenic shock.
In recent years, the rare traditional Chinese medicine resource of the similar genseng of China etc. is come scarcity more, but utilizes the still suitable backwardness of mode.For example, have every year tens of tons of gensengs to be used to produce healthcare products such as panax ginseng extractum, spirit of ginseng, only utilize ginseng effective component's 4%~5% aborning, remaining then goes out of use or as fodder additives, and is very unfortunate.In fact, in the genseng extraction waste material of routine, contain the effective constituent that some have remarkable health-care effect,, then do not obtain reasonable use as the panaxan.
The panaxan is the activeconstituents of Chinese medicine genseng, is the polymer dextran.Panaxan's energy enhancing body immunoloregulation function and the effect of enhancing chemotherapy medicine antitumor have obvious suppression effect (CN200410098413.4) to tumour.The panaxan also has immunoregulation effect in addition, treats viral influenza.At present, the panaxan is a raw material with the genseng crude drug usually, and the method as propositions such as patents (CN200810142918.4, CN200810088971.0 and CN200410000209.4) obtains by a series of extractions and sepn process, and raw materials cost is higher.
Summary of the invention
The invention provides a kind of method that from the red ginseng alcohol extraction waste material, reclaims the panaxan, carry by the red ginseng waste residue after alcohol extracting being carried out water, concentrate, alcohol precipitation, remove technical process such as albumen, vacuum-drying, assay, obtain panaxan's crude product, polysaccharide content is 45%-65% in the crude product, and the yield of polysaccharide reaches more than 10%.
The present invention realizes by following steps:
(1) extraction of genseng Crude polysaccharides:
Getting red ginseng alcohol extracting waste cleans, the pure water that adds 8-15 times of weight then, lixiviate is 2-3 time in 70-100 ℃ of water-bath, each extraction time is 3-4 hour, united extraction liquid, extracting solution is concentrated into the 1/20-1/10 of original volume, adding 95% ethanol (weight percent) then makes the ethanol content of concentrated solution reach 70%-80% (volume percent), in 4 ℃ of refrigerators, left standstill 24-48 hour, centrifuging obtains precipitation, precipitation dehydrated alcohol, acetone repetitive scrubbing, vacuum-drying obtains panaxan's crude product.
(2) panaxan's is refining:
Get the hot water dissolving of panaxan's crude product with 7-10 times of weight, be cooled to room temperature, adopt the Sevag method to remove Deproteinization, centrifugal, obtain polysaccharide liquid, make toward wherein adding 95% ethanol that ethanol content reaches 70%-80% (volume percent) in the polysaccharide liquid, left standstill 24-48 hour at 4 ℃ of refrigerators, centrifuging obtains precipitation, precipitation dehydrated alcohol, acetone repetitive scrubbing, and vacuum-drying obtains the purified panaxan.The vacuum-drying temperature is good with 50-70 ℃.
(3) content Determination of Polysaccharide
Adopt the phenolsulfuric acid colorimetry to measure, phenol concentration is 4%-6% (weight percent), and panaxan's content is 50%-68% in the crude product as a result, and panaxan's yield reaches more than 10%.
Step (2) adopts comparatively gentle Sevag method to remove albumen, promptly adds the chloroform of 1/5 volume earlier in the solution, adds the propyl carbinol of 1/5 chloroform volume again, acutely jolting 20-30 minute.
The present invention proposes the composite extracting method of red ginseng medicinal material, earlier with the red ginseng medicinal material through alcohol extraction process, what obtain medicinal extract mainly contains saponin(e isoreactivity composition, the waste after the alcohol extracting is extracting the panaxan by extraction process by water.The purpose of the compound extraction of red ginseng is: obtain two kinds efficient part from a kind of medicinal material, thereby improve the comprehensive utilization ratio of medicinal material, the ginseng resource of saves valuable.The inventive method is reasonable in design, carries, concentrates, alcohol precipitation, removes methods such as albumen, vacuum-drying by water, and waste residue is fully used, and is suitable for practicality.
Embodiment
The present invention is further described in conjunction with following embodiment.
Embodiment 1:
Accurately take by weighing 50 gram red ginseng alcohol extracting extract remainders, put into the 1000mL round-bottomed flask, add 500mL water respectively, 90 ℃ are extracted twice, and each 4 hours, filter, merging filtrate obtains the filtrate about 950ml.Then, be evaporated to about 90mL at 50-70 ℃.Concentrated solution adds 95% ethanol, makes ethanol content reach 70% (volume percent), places in 4 ℃ of refrigerators and spends the night.Centrifuging obtains precipitation, and precipitation is put into 60 ℃ of vacuum drying ovens dryings more than 12 hours with dehydrated alcohol, acetone repetitive scrubbing, the precipitation that obtains, and obtains genseng Crude polysaccharides product 10.1 grams, and color is greyish white.Get through the phenolsulfuric acid colorimetric method for determining, the content of polysaccharide is 53.8% in this crude product.As calculated, the polysaccharide extract rate of red ginseng alcohol extracting waste is 10.9%.
Embodiment 2:
Accurately take by weighing 50 gram red ginseng alcohol extracting extract remainders, put into the 1000mL round-bottomed flask, add 10 times of water yields, 80 ℃ are extracted twice, each 4 hours, filter merging filtrate, obtain the filtrate about 950mL, be evaporated to about 80ml, in concentrated solution, add 95% ethanol, make ethanol content reach 75% (volume percent), place in 4 ℃ of refrigerators and spend the night, centrifuging obtains precipitation, and precipitation is put into 60 ℃ of vacuum drying ovens dryings more than 12 hours with dehydrated alcohol, acetone repetitive scrubbing, the precipitation that obtains, obtain genseng Crude polysaccharides 10.6 grams, color is a khaki color.Get through assay, the content of polysaccharide is 52.1% in the crude product.Panaxan's yield is 11.1%.
Embodiment 3:
Accurately take by weighing 50 gram red ginseng alcohol extracting waste residues, put into the 1000mL round-bottomed flask, add 10 times of amount 500mL water, 100 ℃ are extracted twice, each 4 hours, filter merging filtrate, obtain the filtrate about 950mL, be evaporated to about 120mL, in concentrated solution, add 95% ethanol, make ethanol content reach 80% (volume percent), place in 4 ℃ of refrigerators and spend the night, centrifuging obtains precipitation, and precipitation is put into 50 ℃ of vacuum drying ovens dryings more than 12 hours with dehydrated alcohol, acetone repetitive scrubbing, the precipitation that obtains, obtain genseng Crude polysaccharides 13.85 grams, color is greyish white.Get through assay, the content of polysaccharide is 56.67% in the crude product.Panaxan's yield is 15.67%.
Embodiment 4:
Accurately take by weighing 50 gram red ginseng alcohol extracting waste residues, put into the 1000mL round-bottomed flask, add 10 times of amount 500mL water, 70 ℃ are extracted twice, each four hours, filter merging filtrate, obtain the filtrate about 950mL, be evaporated to about 100mL, in concentrated solution, add 95% ethanol, make ethanol content reach 72% (volume percent), place in 4 ℃ of refrigerators and spend the night, centrifuging obtains precipitation, and precipitation is put into 50 ℃ of vacuum drying ovens dryings more than 12 hours with dehydrated alcohol, acetone repetitive scrubbing, the precipitation that obtains, obtain genseng Crude polysaccharides 10.29 grams, color is greyish white.Get through assay, the content of polysaccharide is 54% in the crude product, and panaxan's yield is 11.11%.
Embodiment 5:
Get genseng Crude polysaccharides 10 grams that 90 ℃ of extractions obtain, hot water dissolving with 7 times of weight, approximately the polysaccharide soln about 70mL behind the cool to room temperature, removes albumen with the Sevag method, the chloroform that promptly adds 1/5 polysaccharide soln amount earlier, the propyl carbinol that adds 1/5 chloroform amount again, violent then jolting 20 minutes, the centrifugal deproteinize that removes, repeat five times, obtain about polysaccharide liquid 35mL.Adding 95% ethanol makes ethanol content reach 80% (volume percent), spend the night 4 ℃ of refrigerators placements, centrifuging obtains polysaccharide precipitation, with dehydrated alcohol, acetone repetitive scrubbing precipitation, it is dry more than 12 hours that the polysaccharide precipitation that obtains is put into 70 ℃ of vacuum drying ovens, obtain panaxan's highly finished product 5.16 grams, color is greyish white.Get through the phenolsulfuric acid colorimetric method for determining, the content of polysaccharide is 68.8%.

Claims (3)

1. method that reclaims the panaxan from the red ginseng alcohol extraction waste material is characterized in that: realize by following steps:
(1) extraction of genseng Crude polysaccharides:
Getting red ginseng alcohol extracting waste cleans, the pure water that adds 8-15 times of weight then, lixiviate is 2-3 time in 70-100 ℃ of water-bath, and each extraction time is 3-4 hour, united extraction liquid, extracting solution is concentrated into the 1/20-1/10 of original volume, add 95% ethanol then and make the ethanol content of concentrated solution reach 70%-80%, left standstill 24-48 hour in 4 ℃ of refrigerators, centrifuging obtains precipitation, precipitation dehydrated alcohol, acetone repetitive scrubbing, vacuum-drying obtains panaxan's crude product;
(2) panaxan's is refining:
Get the hot water dissolving of panaxan's crude product with 7-10 times of weight, be cooled to room temperature, adopt the Sevag method to remove Deproteinization, centrifugal, obtain polysaccharide liquid, make toward wherein adding 95% ethanol that ethanol content reaches 70%-80% in the polysaccharide liquid, left standstill 24-48 hour at 4 ℃ of refrigerators, centrifuging obtains precipitation, precipitation dehydrated alcohol, acetone repetitive scrubbing, and vacuum-drying obtains the purified panaxan.
(3) content Determination of Polysaccharide
Adopt the phenolsulfuric acid colorimetry to measure, phenol concentration is 4%-6%, and panaxan's content is 50%-68% in the crude product as a result, and panaxan's yield reaches more than 10%.
2. a kind of method that reclaims the panaxan from the red ginseng alcohol extraction waste material according to claim 1 is characterized in that: 50-70 ℃ of the described vacuum-drying temperature of step (2).
3. a kind of method that from the red ginseng alcohol extraction waste material, reclaims the panaxan according to claim 1, it is characterized in that: the described employing of step (2) Sevag method is removed albumen, the last chloroform of adding 1/5 volume in the solution earlier, the propyl carbinol that adds 1/5 chloroform volume again, violent jolting 20-30 minute.
CN2009100982447A 2009-04-30 2009-04-30 Method for recovering Ginseng polysaccharide form red ginseng alcohol extraction waste material Expired - Fee Related CN101550197B (en)

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CN102321188A (en) * 2011-08-17 2012-01-18 哈尔滨怡康药业有限公司 Method for extracting polysaccharides from American ginseng
CN102784181A (en) * 2011-05-17 2012-11-21 天津天士力现代中药资源有限公司 Preparation method of red ginseng polysaccharide
CN102784182A (en) * 2011-05-17 2012-11-21 天津天士力现代中药资源有限公司 Preparation method of Radix Ginseng Rubra polysaccharide extract product
CN102784183A (en) * 2011-05-17 2012-11-21 天津天士力现代中药资源有限公司 Preparation method of red ginseng polysaccharide extract product
CN103053897A (en) * 2011-10-20 2013-04-24 北京以岭药业有限公司 Ginseng polysaccharide chewable tablet and preparation method thereof
CN108424817A (en) * 2018-06-08 2018-08-21 白山市科学技术研究所 A kind of method of processing of Panax ginseng waste extraction ginseng essential oil
CN108619001A (en) * 2018-06-25 2018-10-09 上海交通大学医学院 A kind of red ginseng facial mask and preparation method thereof of preservative free addition
CN114748584A (en) * 2022-05-05 2022-07-15 浙江工业大学 Dendrobium officinale composition capable of enhancing immunity by improving levels of complements C3 and C4 and preparation method and application thereof

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CN100457119C (en) * 2006-03-30 2009-02-04 汤玉生 Freeze dried ginseng polysaccharide powder for injection and its preparing process
CN1821275A (en) * 2006-04-07 2006-08-23 吉林省宏久生物科技股份有限公司 Ginseng extracting method for separating ginseng polyose and extract and use of ginseng polyose
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CN102784181A (en) * 2011-05-17 2012-11-21 天津天士力现代中药资源有限公司 Preparation method of red ginseng polysaccharide
CN102784182A (en) * 2011-05-17 2012-11-21 天津天士力现代中药资源有限公司 Preparation method of Radix Ginseng Rubra polysaccharide extract product
CN102784183A (en) * 2011-05-17 2012-11-21 天津天士力现代中药资源有限公司 Preparation method of red ginseng polysaccharide extract product
CN102784181B (en) * 2011-05-17 2016-06-15 天津天士力现代中药资源有限公司 The preparation method of a kind of red gracilis polysaccharide
CN102784183B (en) * 2011-05-17 2016-06-15 天津天士力现代中药资源有限公司 The preparation method of a kind of Radix Ginseng Rubra polysaccharide extract product
CN102321188A (en) * 2011-08-17 2012-01-18 哈尔滨怡康药业有限公司 Method for extracting polysaccharides from American ginseng
CN103053897A (en) * 2011-10-20 2013-04-24 北京以岭药业有限公司 Ginseng polysaccharide chewable tablet and preparation method thereof
CN103053897B (en) * 2011-10-20 2016-09-28 北京以岭药业有限公司 A kind of ginseng polysaccharide chewable tablet and preparation method thereof
CN108424817A (en) * 2018-06-08 2018-08-21 白山市科学技术研究所 A kind of method of processing of Panax ginseng waste extraction ginseng essential oil
CN108619001A (en) * 2018-06-25 2018-10-09 上海交通大学医学院 A kind of red ginseng facial mask and preparation method thereof of preservative free addition
CN108619001B (en) * 2018-06-25 2021-09-07 上海交通大学医学院 Red ginseng mask without preservative and preparation method thereof
CN114748584A (en) * 2022-05-05 2022-07-15 浙江工业大学 Dendrobium officinale composition capable of enhancing immunity by improving levels of complements C3 and C4 and preparation method and application thereof

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