CN1112366C - Extraction of gensenoside - Google Patents
Extraction of gensenoside Download PDFInfo
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- CN1112366C CN1112366C CN 00110418 CN00110418A CN1112366C CN 1112366 C CN1112366 C CN 1112366C CN 00110418 CN00110418 CN 00110418 CN 00110418 A CN00110418 A CN 00110418A CN 1112366 C CN1112366 C CN 1112366C
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Abstract
The present invention discloses a method for extracting total ginsenosides. The method comprises the following processing steps: using water as an initial solvent; soaking and decocting ginseng; filtering slag out and taking filtrate; decompressing and concentrating the filtrate; obtaining eluent after a concentrated solution is adsorbed by a macroporous resin column and eluted by ethanol; adding magnesium oxide to the eluent; heating the eluent for reflux and decolorization; collecting filtrate; eliminating impurities in the filtrate by using exchange resin; finally, recovering the ethanol in the filtrate and drying remanent substances to obtain a final product. Compared with the prior art, the present invention after realization has the advantages of low cost, little impurity, no pollution to environment in production process, etc.
Description
The present invention relates to the extracting method of plant total saponins, exactly is the extracting method of Radix Ginseng total saponins.
Radix Ginseng total saponins not only can be used as the additive of products such as food, makeup, feed, but also can be used as multiple medicine as a kind of physiologically active substance, and the preparation raw material of various healthcare products is used very extensive.Because the Radix Ginseng total saponins product has high using value, so in the last few years, the expert who comprises many countries of China, the scholar is to from genseng, particularly the method for extracting Radix Ginseng total saponins from root, stem, leaf, fruit and the reed head of genseng has been carried out extensive and deep research, obtains gratifying achievement.Wherein, the extracting method of day Radix Ginseng total saponins of the present disclosure has certain representativeness.For example, when ginseng material was selected the Ginseng Leaf for use, the technological process of utilizing this method to extract Radix Ginseng total saponins was: make starting solvent soaking ginseng material and refluxing extraction 8 times with methyl alcohol, again reclaim under reduced pressure methyl alcohol; After adding water, with n-butanol extraction 8 times and reclaim under reduced pressure propyl carbinol; Medicinal extract concentration is 95% dissolve with ethanol, and makes it pass through aluminium sesquioxide chromatography column and active carbon column; Collect effluent liquid and reclaim under reduced pressure, make finished product.The subject matter of utilizing this method to produce the ginsenoside existence is: 1, product cost is higher, and per kilogram finished product cost is up to 1200 yuans; 2, the impurity in the product, particularly content of harmful is higher, and wherein heavy metal content surpasses 5PPm, and pesticide residue surpasses prescribed limit greater than 10PPb, simultaneously residual toxicity solvent, n-butanol etc. inevitably also.
The objective of the invention is to provide for people a kind of extracting method of new Radix Ginseng total saponins, so that make the Radix Ginseng total saponins cost that utilizes this method to produce low, foreign matter content is few, and makes its production process environmentally safe,
The method for preparing Radix Ginseng total saponins provided by the invention comprises following processing step:
A, ginseng material soak and decoct
(A) ratio of weight and number by ginseng material and tap water is 1: 8-16 adds tap water in the ginseng material, and soak at room temperature 0.5-2 hour, then, the mixture heating up to 70 ℃-100 ℃ with both was incubated 1-3 hour, afterwards, and residue obtained liquid;
(B) ratio of weight and number by described ginseng material and tap water is 1: 6-10 adds tap water in the slag that work step (A) leaches, and with both mixture heating up to 70 ℃-100 ℃, is incubated 1-2.5 hour, afterwards, and residue obtained liquid;
(C) ratio of weight and number by described ginseng material and tap water is 1: 6-8 adds tap water in the slag that work step (B) leaches, and with both mixture heating up to 70 ℃-100 ℃, is incubated 1-1.5 hour, afterwards, and residue obtained liquid;
B, liquid concentration
The liquid mixing that will be respectively produce by described each work step (A), (B), (C) is the back concentrating under reduced pressure together, and be 1-3 until the ratio of its weight and described ginseng material weight: 1 ends;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, saponin(e in the liquid is adsorbed by resin column, and discard effluent liquid, the ratio of the volume of liquid is 0.1-1 with concentrating afterwards in distilled water again: 1 ratio is taken the distilled water flushing resin column, discard effluent liquid, continuing with concentration is the ethanol cleaning resin column of 50-70%, absorption saponin(e is thereon ended by complete wash-out, and collect elutriant;
D, decolouring
Ratio of weight and number in medicinal magnesium oxide and described ginseng section is 2-6: 100 ratio is taken medicinal magnesium oxide and is added in the described elutriant, reflux 20-60 minute, then, this mixture is filtered by clear slag plate, and collects filtrate;
E, impurity elimination
Described filtering is passed through in the Zeo-karb that is one another in series and anionite-exchange resin, made wherein ion and heavy metal by filtering, and collection filtrate;
F, finished product reclaim, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Radix Ginseng total saponins finished product.
Compared with the prior art the present invention has the following advantages after realizing: 1, cost is low, and the per kilogram cost is 600 yuans; 2, heavy metal content is less than 5PPm in the finished product, and pesticide residue is less than 10PPb, thereby its foreign matter content is low; 3, elimination toxicant propyl carbinol is residual; 4, production process environmentally safe.
Embodiment one
A, immersion and decoction
(A) get and have the ginseng 1kg that is about 5-8% reed head and put into container, in container, add 8 liters in tap water again, soak at room temperature 1 hour, then, the mixture heating up to 70 ℃-80 ℃ with both is incubated 3 hours, afterwards, residue obtained liquid;
(B) in the slag that work step (A) leaches, add 6 liters in tap water, and, be incubated 2 hours both mixture heating up to 70 ℃-80 ℃, afterwards, residue obtained liquid;
(C) in the slag that work step (B) leaches, add 6 liters in tap water, and, be incubated 1.5 hours both mixture heating up to 70 ℃-80 ℃, afterwards, residue obtained liquid;
B, liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by above-mentioned each work step (A), (B), (C) respectively is concentrated into about 3 until it and only is upgraded to;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, saponin(e in the liquid is adsorbed by resin column, and discard effluent liquid, use 3 liters of distilled water flushing resin columns again, discard effluent liquid, continuing with concentration is that 70% ethanol cleans resin column, absorption saponin(e is thereon ended by wash-out fully, and collect elutriant;
D, decolouring
Content being not less than 97% the medicinal light magnesium oxide 0.03kg that meets Chinese Pharmacopoeia (II portion) required standard adds in the described elutriant, be heated to 70-80 ℃, and both mixtures refluxed 45 minutes, then at this temperature condition, this mixture is filtered by clear slag plate, and collect filtrate;
E, impurity elimination
Described filtrate is passed through in the 732 type Zeo-karbs that are one another in series and 717 type anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F, finished product reclaim, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Radix Ginseng total saponins finished product.
Produce the Radix Ginseng total saponins product by the present embodiment method:
1, yield (weight percent) is 3.5-4.8%.
2, " colorimetry " put down in writing by " Shenyang Pharmacy College's journal " the 25th phase 288-291 page or leaf of publication in 1985 detects the content of this product 〉=90%.
3, press the HPLC method and detect the contained Re of this product, Rg
1, Rc, Rd, Rb
1, Rh
1Six kinds of saponin content sum 〉=60%.
4, composition: isolation identification totally 19 kinds of saponin(es, be respectively ginsenoside R0, Ra
1, Ra
2, Rb
1, Rb
2, Rc, Rd, Re, Rg
1, Rg
2, Rg
3, Rg
4, Rh, Rh
1, Rh
2, Rh
3, Rf, R20 (Glc)-Rf, Rd
2
5, foreign matter content: heavy metal≤5PPm, pesticide residue, promptly the residual quantity of " 666 ", " DDT ", " 5 chloronitrobenzene " all≤10PPb.
Embodiment two
A, immersion and decoction
(A) get Radix Ginseng stem and leaf 10kg puts into container, in container, add 160 liters in tap water again, soak at room temperature 2 hours, then, the mixture heating up to 95 ℃-100 ℃ with both is incubated 2.5 hours, afterwards, residue obtained liquid;
(B) in the slag that work step (A) leaches, add 100 liters in tap water, and, be incubated 2.5 hours both mixture heating up to 95 ℃-100 ℃, afterwards, residue obtained liquid;
(C) in the slag that work step (B) leaches, add 80 liters in tap water, and, be incubated 1 hour both mixture heating up to 95 ℃-100 ℃, afterwards, residue obtained liquid;
B, liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by above-mentioned each work step (A), (B), (C) respectively is concentrated into about 20 until it and only is upgraded to;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, saponin(e in the liquid is adsorbed by resin column, and discard effluent liquid, use 16 liters of distilled water flushing resin columns again, discard effluent liquid, continuing with concentration is that 60% ethanol cleans resin column, absorption saponin(e is thereon ended by wash-out fully, and collect elutriant;
D, decolouring
Content is not less than 97% the medicinal light magnesium oxide 0.6kg that meets Chinese Pharmacopoeia (II portion) required standard and adds in the described elutriant, reflux 60 minutes then, makes this mixture filter by clear slag plate, and collects filtrate;
E, impurity elimination
Described filtrate is passed through in the 732 type Zeo-karbs that are one another in series and 717 type anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F, finished product reclaim, drying
Recovery process E makes the ethanol in the filtrate, and remaining material can obtain the Radix Ginseng total saponins finished product after passing through reduced vacuum drying or spraying drying mode drying.
Produce the Radix Ginseng total saponins product by the present embodiment method:
1, yield (weight percent) is 4.8-5.2%.
2, " colorimetry " put down in writing by " Shenyang Pharmacy College's journal " the 25th phase 288-291 page or leaf of publication in 1985 detects the content of this product 〉=90%
3, press the HPLC method and detect the contained Re of this product, Rg
1, Rc, Rd, Rb
1, Rh
1Six kinds of saponin content sum 〉=60%.
4, composition: isolation identification totally 19 kinds of saponin(es, be respectively the ginsenoside Ra
0, Rb
1, Rb
2, Rb
3, Rc, Rd, Rf, Re, Rg
1, Rg
2, Rg
3, Rh
1, Rh
2, Rh
3, RLa, F4,25-hydroxyl stem-Protopanaxatriol, 25-hydroxyl stem ginsenoside Rg
2, the Ginsenoside Rd
2, wherein back 6 kinds is new compound.
5, foreign matter content: heavy metal≤5PPm, pesticide residue, promptly the residual quantity of " 666 ", " DDT ", " 5 chloronitrobenzene " all≤10PPb.
Embodiment three
A, immersion and decoction
(A) get ginseng flower bud 10kg and put into container, in container, add 150 liters in tap water again, soak at room temperature 0.5 hour, then, the mixture heating up to 80 ℃-90 ℃ with both is incubated 1 hour, afterwards, residue obtained liquid;
(B) in the slag that work step (A) leaches, add 100 liters in tap water, and, be incubated 1 hour both mixture heating up to 95 ℃-100 ℃, afterwards, residue obtained liquid;
(C) in the slag that work step (B) leaches, add 80 liters in tap water, and, be incubated 1 hour both mixture heating up to 95 ℃-100 ℃, afterwards, residue obtained liquid;
B, liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by above-mentioned each work step (A), (B), (C) respectively is concentrated into about 10 until it and only is upgraded to;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, saponin(e in the liquid is adsorbed by resin column, and discard effluent liquid, use 1 liter of distilled water flushing resin column again, discard effluent liquid, continuing with concentration is that 50% ethanol cleans resin column, absorption saponin(e is thereon ended by wash-out fully, and collect elutriant;
D, decolouring
Content is not less than 97% the medicinal light magnesium oxide 0.2kg that meets Chinese Pharmacopoeia (II portion) required standard and adds in the described elutriant, reflux 30 minutes then, makes this mixture filter by clear slag plate, and collects filtrate;
E, impurity elimination
Described filtrate is passed through in the 732 type Zeo-karbs that are one another in series and 717 type anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F, finished product reclaim, drying
Recovery process E makes the ethanol in the filtrate, and remaining material can obtain the Radix Ginseng total saponins finished product after passing through reduced vacuum drying or spraying drying mode drying.
Produce the Radix Ginseng total saponins product by the present embodiment method:
1, yield (weight percent) is 5.0-5.5%.
2, " colorimetry " put down in writing by " Shenyang Pharmacy College's journal " the 25th phase 288-291 page or leaf of publication in 1985 detects the content of this product 〉=90%
3, press the HPLC method and detect the contained Re of this product, Rg
1, Rc, Rd, Rb
1, Rh
1Six kinds of saponin content sum 〉=60%.
4, composition: isolation identification totally 18 kinds of saponin(es, be respectively ginsenoside Ra 0, Rb
1, Rb
2, Rc, Rd, Rf, Re, Rg
1, Rg
2, Rg
3, Rh
1, Rh
2, Rh
3, Rd
2, F4,25-hydroxyl stem-protopanoxadiol, 25-hydroxyl stem ginsenoside Rg
2
5, foreign matter content: heavy metal≤5PPm, pesticide residue, promptly the residual quantity of " 666 ", " DDT ", " 5 chloronitrobenzene " all≤10PPb.
Claims (1)
1, the extracting method of Radix Ginseng total saponins, form by following processing step:
A, ginseng material soak and decoct
(A) ratio of weight and number by ginseng material and tap water is 1: 8-16 adds tap water in the ginseng material, and soak at room temperature 0.5-2 hour, then, the mixture heating up to 70 ℃-100 ℃ with both was incubated 1-3 hour, afterwards, and residue obtained liquid;
(B) ratio of weight and number by described ginseng material and tap water is 1: 6-10 adds tap water in the slag that work step (A) leaches, and with both mixture heating up to 70 ℃-100 ℃, is incubated 1-2.5 hour, afterwards, and residue obtained liquid;
(C) ratio of weight and number by described ginseng material and tap water is 1: 6-8 adds tap water in the slag that work step (B) leaches, and with both mixture heating up to 70 ℃-100 ℃, is incubated 1-1.5 hour, afterwards, and residue obtained liquid;
B, liquid concentration
The liquid mixing that will be respectively produce by described each work step (A), (B), (C) is the back concentrating under reduced pressure together, and be 1-3 until the ratio of its weight and described ginseng material weight: 1 ends;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, saponin(e in the liquid is adsorbed by resin column, and discard effluent liquid, the ratio of the volume of liquid is 0.1-1 with concentrating afterwards in distilled water again: 1 ratio is taken the distilled water flushing resin column, discard effluent liquid, continuing with concentration is the ethanol cleaning resin column of 50-70%, absorption saponin(e is thereon ended by complete wash-out, and collect elutriant;
D, decolouring
Ratio of weight and number in medicinal magnesium oxide and described ginseng material is 2-6: 100 ratio is taken medicinal magnesium oxide and is added in the described elutriant, reflux 20-60 minute, then, this mixture is filtered by clear slag plate, and collects filtrate;
E, impurity elimination
Described filtrate is passed through in the Zeo-karb that is one another in series and anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F, finished product reclaim, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Radix Ginseng total saponins finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110418 CN1112366C (en) | 2000-05-17 | 2000-05-17 | Extraction of gensenoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110418 CN1112366C (en) | 2000-05-17 | 2000-05-17 | Extraction of gensenoside |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1277205A CN1277205A (en) | 2000-12-20 |
| CN1112366C true CN1112366C (en) | 2003-06-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00110418 Expired - Fee Related CN1112366C (en) | 2000-05-17 | 2000-05-17 | Extraction of gensenoside |
Country Status (1)
| Country | Link |
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| CN (1) | CN1112366C (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1296379C (en) * | 2005-06-03 | 2007-01-24 | 吉林农业大学 | Technique for preparing malonyl ginsenoside, and application of medication in treating diabetes |
| CN101084955B (en) * | 2006-06-08 | 2012-02-01 | 天津天士力之骄药业有限公司 | Method for preparing total ginsenoside |
| CN101084954B (en) * | 2006-06-08 | 2012-02-01 | 天津天士力之骄药业有限公司 | Method for preparing American ginseng total saponins |
| CN1869052B (en) * | 2006-06-21 | 2013-03-06 | 海南亚洲制药有限公司 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
| CN102772462B (en) * | 2011-05-11 | 2016-08-24 | 河北以岭医药研究院有限公司 | A kind of method extracting separation Radix Ginseng total saponins from Radix Panacis Quinquefolii |
| CN102488251B (en) * | 2011-12-12 | 2013-04-03 | 中国海洋大学 | Sea cucumber gelatin, preparation method thereof, medicine or health product containing sea cucumber gelatin, and application of sea cucumber gelatin |
| CN102618616B (en) * | 2012-04-13 | 2013-09-11 | 吉林农业大学 | Method of improving ginsenoside extraction rate by utilizing steam-explosion combined bio-composite enzyme technology |
| CN102727548A (en) * | 2012-07-03 | 2012-10-17 | 吉林省宏久生物科技股份有限公司 | New technology and method for extracting ginseng stem and leaf total saponin |
| CN102846685A (en) * | 2012-09-25 | 2013-01-02 | 吉林省宏久生物科技股份有限公司 | Preparation technology and method for improving total content of ginseng saponin through fermentation method |
| CN104415070B (en) * | 2013-08-30 | 2019-06-25 | 河北以岭医药研究院有限公司 | A kind of isolation and purification method of Ginsenosides in Panax Ginseng |
| CN103960568B (en) * | 2014-05-29 | 2016-05-25 | 延边长白山药业有限公司 | A kind of general ginsenoside chewable tablets and preparation method thereof |
| CN105852130A (en) * | 2016-05-24 | 2016-08-17 | 朱启标 | Preparation method of ginseng health care product and product of preparation method |
| CN106153810A (en) * | 2016-07-27 | 2016-11-23 | 长春中医药大学 | A kind of preparation method and application of stem and leaf of Radix Ginseng total saponins reference extract |
| CN106805243A (en) * | 2017-02-28 | 2017-06-09 | 吉林省清评科技有限公司 | A kind of high-valued method of comprehensive utilization of Ginseng under Forest |
| CN108524564A (en) * | 2018-03-08 | 2018-09-14 | 安徽九华华源药业有限公司 | The extracting method of ginseng seed's total saposins |
| CN113116946A (en) * | 2019-12-30 | 2021-07-16 | 天津天士力现代中药资源有限公司 | Method for simultaneously preparing red ginseng fibrous root polysaccharide and saponin extraction |
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2000
- 2000-05-17 CN CN 00110418 patent/CN1112366C/en not_active Expired - Fee Related
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|---|---|
| CN1277205A (en) | 2000-12-20 |
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Owner name: JINLIN CHANGQING GINSENG CO., LTD. Free format text: FORMER OWNER: XU SUIXU Effective date: 20120308 |
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Effective date of registration: 20120308 Address after: Ji'an City, Jilin province 134200 Ma Xian Xiang Huo Long Cun. Co-patentee after: Yang Shiming Patentee after: Jilin evergreen ginseng industry Co., Ltd. Address before: 110015 No. 103, Wenhua Road, Shenhe District, Liaoning, Shenyang Co-patentee before: Liu Shuqin Patentee before: Xu Suixu Co-patentee before: Yang Shiming |
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