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 PDFInfo
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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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- Prior art keywords
- panaxan
- polysaccharide
- red ginseng
- ginseng
- alcohol extraction
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 150000004676 glycans Polymers 0.000 title claims abstract description 32
- 235000002789 Panax ginseng Nutrition 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002699 waste material Substances 0.000 title claims abstract description 21
- 235000008434 ginseng Nutrition 0.000 title abstract description 10
- 241000208340 Araliaceae Species 0.000 title abstract description 9
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 title abstract description 8
- 235000003140 Panax quinquefolius Nutrition 0.000 title abstract description 8
- 150000004804 polysaccharides Polymers 0.000 title abstract 2
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 30
- 239000005017 polysaccharide Substances 0.000 claims abstract description 30
- 239000012043 crude product Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 229960004756 ethanol Drugs 0.000 claims description 18
- 238000001291 vacuum drying Methods 0.000 claims description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 230000003252 repetitive effect Effects 0.000 claims description 9
- 238000005201 scrubbing Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 102000011759 adducin Human genes 0.000 claims description 4
- 108010076723 adducin Proteins 0.000 claims description 4
- 238000004737 colorimetric analysis Methods 0.000 claims description 4
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000003544 deproteinization Effects 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 238000001035 drying Methods 0.000 abstract description 5
- 229930182490 saponin Natural products 0.000 abstract description 2
- 150000007949 saponins Chemical class 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 102000004169 proteins and genes Human genes 0.000 abstract 1
- 108090000623 proteins and genes Proteins 0.000 abstract 1
- 235000017709 saponins Nutrition 0.000 abstract 1
- 238000003809 water extraction Methods 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 description 8
- 239000003814 drug Substances 0.000 description 7
- 206010013786 Dry skin Diseases 0.000 description 4
- 238000003556 assay Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 240000004371 Panax ginseng Species 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 206010019280 Heart failures Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010033557 Palpitations Diseases 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 206010007625 cardiogenic shock Diseases 0.000 description 1
- 238000002512 chemotherapy Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000002519 immonomodulatory effect Effects 0.000 description 1
- 230000007365 immunoregulation Effects 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- 230000003612 virological effect Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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
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.
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