CN110105459A - A kind of extracting method of notoginseng polysaccharide - Google Patents
A kind of extracting method of notoginseng polysaccharide Download PDFInfo
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- CN110105459A CN110105459A CN201910443332.XA CN201910443332A CN110105459A CN 110105459 A CN110105459 A CN 110105459A CN 201910443332 A CN201910443332 A CN 201910443332A CN 110105459 A CN110105459 A CN 110105459A
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- polysaccharide
- notoginseng
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Abstract
The present invention relates to field of medicine preparing technology, and in particular to a kind of extracting method of notoginseng polysaccharide.Method includes the following steps: A), extract: take Radix Notoginseng bulk medicinal material, ethyl alcohol be added, pour into wet type pulverizing mill crush and collect filtrate；B), it is centrifuged: the filtrate of collection is separated by centrifuge；C), it is concentrated in vacuo, extracting solution is made；D), refine；It will obtain that purified water dissolution is added in extracting solution, trifluoromethanesulfonic acid is then added, obtains liquid of extracting polysaccharide；E), chromatograph: resin cation is added in liquid of extracting polysaccharide, is washed with purified water, and combination system obtains eluent；F), purify: G), being concentrated: notoginseng polysaccharide solution is first depressurized to pour into n-butanol and be stood after stirring, and notoginseng polysaccharide crystalline deposit object is made after layering；H), notoginseng polysaccharide is made by being dried in vacuo.Present invention solution has in existing extracting method, and notoginseng polysaccharide recovery rate is low and the high problem of impurity content, and can improve product quality.
Description
Technical field
The present invention relates to field of medicine preparing technology, and in particular to a kind of extracting method of notoginseng polysaccharide.
Background technique
Radix Notoginseng also known as invaluable is Araliaceae, with its root as medicinal effects.Radix Notoginseng main product is in Yunnan Province of China text
The ground such as mountain, notoginseng polysaccharide be extracted from Radix Notoginseng there is multiple biological activities and complicated heteroglycan or its is compound
Object.Numerous studies prove that notoginseng polysaccharide has the multiple efficacies such as antitumor, hypoglycemic, anti-oxidant, strengthen immunity.Current three
Seven extraction method of polysaccharides generally use solvent reflux extraction to extract preparation, and this method has notoginseng polysaccharide in final extract more
The problem of content is relatively low, and the production cycle is long, and energy consumption cost increases, and due to being to extract under the high temperature conditions, also cause
The impurity contents such as ash content are excessively high, unstable product quality.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of extracting methods of the notoginseng polysaccharide of reliable performance, have solved
In existing extracting method, notoginseng polysaccharide recovery rate is low and the high problem of impurity content, and can improve product quality.
The technical scheme of the present invention is realized as follows: a kind of extracting method of notoginseng polysaccharide, comprising the following steps:
A), extract:
Radix Notoginseng bulk medicinal material is taken, 70% ethyl alcohol is added, is subsequently poured into wet type pulverizing mill and is crushed, grinding time 8
~30min, then filters and collects filtrate；
B), it is centrifuged: the filtrate of collection is separated by centrifuge, and centrifugate is made；
C), it is concentrated in vacuo: by centrifugate by automatic concentration device retraction volume, extracting solution is made, extracting solution is dense to depressurize
It is reduced to 8~10 ° of Baume degrees；
D), refine；It will obtain that purified water dissolution is added in extracting solution, the fluoroform of mixture quality 4~6% is then added
Sulfonic acid, after 90~95 DEG C of 20~30min of closed hydrolysis, vacuum recycling trifluoromethanesulfonic acid obtains polysaccharide and slightly mentions at 45~65 DEG C
Liquid；
E), chromatograph: resin cation is added in liquid of extracting polysaccharide, is washed with purified water, and combination system obtains eluent；
F), purify: eluent first being poured into alumina column adsorption bleaching, then is placed in reaction kettle, 3~5% activity are added
Powdered carbon, impregnates 20min at 50~60 DEG C after mixing, and with obtaining notoginseng polysaccharide solution after stud filter refined filtration；
G), be concentrated: notoginseng polysaccharide solution is first concentrated under reduced pressure into 15~20 ° of Baume degrees, pours into n-butanol after stirring and stands,
N-butanol layer is separated after layering, is reduced to 20~25 ° of Baume degrees in decompression, and notoginseng polysaccharide crystalline deposit object is made；
H), dry: purified water being added in sediment, adjusts density, by vacuum drying 2~3 hours, it is more that Radix Notoginseng is made
Sugar.
Preferably, in the step A, the ethanol solution quality of addition is 8~12 times of Radix Notoginseng quality.
0.25~0.4 micron of the filter element filtering precision of the stud filter.
Preferably, in the step E, resin cation and liquid of extracting polysaccharide mass ratio are 3~4:1, are carried out with purified water
When washing, the volume ratio of purified water and resin cation is 9:1, and the flow velocity for being passed through purified water is 300~350L/h.
Preferably, in the step H, it is 1.02~1.15 that purified water adjustment density is added in sediment, drying temperature
Not less than 85 DEG C, vacuum degree is not less than -0.1mpa.
The invention solves the defect existing in the background technology, has the advantages that
Present invention solution has in existing extracting method, and notoginseng polysaccharide recovery rate is low and the high problem of impurity content, and can mention
High yield quality.For the present invention by extracting after Radix Notoginseng is pulverized 10min with 70% ethyl alcohol, notoginseng polysaccharide content is higher.It is logical
It crosses trifluoromethanesulfonic acid and carries out polysaccharide molecule control hydrolysis reaction, so that macromolecular polysaccharide turns to the hydrolysis of micromolecular polysaccharide direction
Change, more mild more controllable than traditional enzymatic hydrolysis reaction, micromolecular polysaccharide absorptivity is higher, to improve the recovery rate of polysaccharide.It is logical
Pigment is sloughed in the absorption of peroxidating aluminium column, and it is miscellaneous that activated carbon powder and resin cation slough amino acid, protein, ash content in liquid etc.
Matter solves the problems, such as that gained polysaccharide ash content is exceeded in conventional method, has better commercial operability.
Detailed description of the invention
Fig. 1 is particle diameter distribution when pulverizing different time；
Specific embodiment
Comparative examples
1000g Radix Notoginseng bulk medicinal material is taken, is extracted according to traditional using solvent reflux extraction preparation, it is more to measure its Radix Notoginseng
Sugared content, content of beary metal and content of ashes, are made data, as comparative examples.
Embodiment 1
Radix Notoginseng bulk medicinal material 1000g is taken, 30% ethyl alcohol is added, is subsequently poured into wet type pulverizing mill and is crushed, is crushed
Time 8min, then filters and collects filtrate, and the ethanol solution quality of addition is 8 times of Radix Notoginseng quality.The filtrate of collection is led to
It crosses centrifuge to be separated, and centrifugate is made；By centrifugate by automatic concentration device retraction volume, extracting solution is made, extracts
Liquid is to be concentrated under reduced pressure into 8~10 ° of Baume degrees；Purified water dissolution is added in obtaining extracting solution, mixture quality 4% is then added
Trifluoromethanesulfonic acid, after 90 DEG C of closed hydrolysis 20min, vacuum recycling trifluoromethanesulfonic acid obtains polysaccharide and slightly mentions at 45~65 DEG C
Liquid；Resin cation is added in liquid of extracting polysaccharide, is washed with purified water, and combination system obtains eluent.Resin cation with
Liquid of extracting polysaccharide mass ratio is 3:1, and when being washed with purified water, the volume ratio of purified water and resin cation is 9:1, is passed through
The flow velocity of purified water is 300L/h.Eluent is first poured into alumina column adsorption bleaching, then is placed in reaction kettle, it is living to be added 3%
Property powdered carbon, impregnates 20min at 50~60 DEG C after mixing, and with obtaining notoginseng polysaccharide solution after stud filter refined filtration.Radix Notoginseng is more
Sugar juice is first concentrated under reduced pressure into 15 ° of Baume degrees, pours into n-butanol after stirring and stands, n-butanol layer is separated after layering, is being depressurized
20 ° of Baume degrees are reduced to, notoginseng polysaccharide crystalline deposit object is made；Purified water is added in sediment, adjusts density, it is dry by vacuum
Dry 2 hours, notoginseng polysaccharide is made, measures its Radix Notoginseng polyoses content, content of beary metal and content of ashes, the number of embodiment 1 is made
According to.
Embodiment 2
Radix Notoginseng bulk medicinal material 1000g is taken, 70% ethyl alcohol is added, is subsequently poured into wet type pulverizing mill and is crushed, is crushed
Time 10min, then filters and collects filtrate, and the ethanol solution quality of addition is 10 times of Radix Notoginseng quality.By the filtrate of collection
It is separated by centrifuge, and centrifugate is made；By centrifugate by automatic concentration device retraction volume, extracting solution is made, mentions
Liquid is taken to be concentrated under reduced pressure into 9 ° of Baume degrees；Purified water dissolution is added in obtaining extracting solution, mixture quality 5% is then added
Trifluoromethanesulfonic acid, after 90~95 DEG C of closed hydrolysis 25min, vacuum recycling trifluoromethanesulfonic acid obtains polysaccharide and slightly mentions at 45~65 DEG C
Liquid；Resin cation is added in liquid of extracting polysaccharide, is washed with purified water, and combination system obtains eluent.Resin cation with
Liquid of extracting polysaccharide mass ratio is 3.5:1, and when being washed with purified water, the volume ratio of purified water and resin cation is 9:1, is led to
The flow velocity for entering purified water is 320L/h.Eluent is first poured into alumina column adsorption bleaching, then is placed in reaction kettle, is added 4%
Active powdered carbon, impregnates 20min at 50~60 DEG C after mixing, and with obtaining notoginseng polysaccharide solution after stud filter refined filtration.Radix Notoginseng
Polysaccharide solution is first concentrated under reduced pressure into 18 ° of Baume degrees, pours into n-butanol after stirring and stands, n-butanol layer is separated after layering, is being subtracted
22 ° of Baume degrees are compressed to, notoginseng polysaccharide crystalline deposit object is made；Purified water is added in sediment, adjusts density, passes through vacuum
It is 2.5 hours dry, notoginseng polysaccharide is made, measures its Radix Notoginseng polyoses content, content of beary metal and content of ashes, embodiment 2 is made
Data.
Embodiment 3
Radix Notoginseng bulk medicinal material 1000g is taken, 90% ethyl alcohol is added, is subsequently poured into wet type pulverizing mill and is crushed, is crushed
Time 30min, then filters and collects filtrate；The ethanol solution quality of addition is 12 times of Radix Notoginseng quality.By the filtrate of collection
It is separated by centrifuge, and centrifugate is made；By centrifugate by automatic concentration device retraction volume, extracting solution is made, mentions
Liquid is taken to be concentrated under reduced pressure into 10 ° of Baume degrees；Purified water dissolution is added in obtaining extracting solution, mixture quality 6% is then added
Trifluoromethanesulfonic acid, after 90~95 DEG C of closed hydrolysis 30min, to obtain polysaccharide thick for vacuum recycling trifluoromethanesulfonic acid at 45~65 DEG C
Extract；Resin cation is added in liquid of extracting polysaccharide, is washed with purified water, and combination system obtains eluent.Resin cation
It is 4:1 with liquid of extracting polysaccharide mass ratio, when being washed with purified water, the volume ratio of purified water and resin cation is 9:1, is led to
The flow velocity for entering purified water is 350L/h.Eluent is first poured into alumina column adsorption bleaching, then is placed in reaction kettle, is added 5%
Active powdered carbon, impregnates 20min at 50~60 DEG C after mixing, and with obtaining notoginseng polysaccharide solution after stud filter refined filtration.Radix Notoginseng
Polysaccharide solution is first concentrated under reduced pressure into 20 ° of Baume degrees, pours into n-butanol after stirring and stands, n-butanol layer is separated after layering, is being subtracted
25 ° of Baume degrees are compressed to, notoginseng polysaccharide crystalline deposit object is made；Purified water is added in sediment, adjusts density, passes through vacuum
It is 3 hours dry, notoginseng polysaccharide is made, measures its Radix Notoginseng polyoses content, content of beary metal and content of ashes, embodiment 3 is made
Data.
Reference examples, the embodiment of the present invention 1, embodiment 2 and embodiment 3 are compared, can obviously be obtained, the present invention mentions
The method of confession can greatly improve the extracted amount of notoginseng polysaccharide.Radix Notoginseng is higher with 70% ethyl alcohol extraction 15min efficiency, by Fig. 1 institute
Show, it can be seen that with pulverizing, 10min extraction effect is preferable, and 100 μm or so of most of Radix Notoginseng granularity, cell is substantially broken
It is broken, and recovery rate highest, when more than 30min, since Radix Notoginseng partial size reduces, surface be can increase, and it is more to have adsorbed a part of Radix Notoginseng
Sugar declines polysaccharide extract rate instead.The present invention pulverizes the more common circumfluence method of method recovery rate using wet type and greatly improves, general
Logical circumfluence method needs 2 hours, and wet type pulverizes method and only needs 10 minutes, and easy to operate, temperature control, crushes and extracts
It synchronously completes.Polysaccharide molecule is carried out by trifluoromethanesulfonic acid and controls hydrolysis reaction, so that macromolecular polysaccharide is more to small molecule
Sugared direction hydrolysis, more mild more controllable than traditional enzymatic hydrolysis reaction, micromolecular polysaccharide absorptivity is higher, to improve polysaccharide
Recovery rate.Pigment is sloughed by alumina column absorption, activated carbon powder and resin cation slough amino acid, albumen in liquid
The impurity such as matter, ash content, solve the problems, such as in conventional method polysaccharide ash content it is exceeded, there is better commercial operability.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of extracting method of notoginseng polysaccharide, it is characterised in that: the following steps are included:
A), extract:
Radix Notoginseng bulk medicinal material is taken, 70% ethyl alcohol is added, is subsequently poured into wet type pulverizing mill and is crushed, grinding time 8~
Then 30min is filtered and is collected filtrate；
B), it is centrifuged: the filtrate of collection is separated by centrifuge, and centrifugate is made；
C), it is concentrated in vacuo: by centrifugate by automatic concentration device retraction volume, extracting solution is made, extracting solution is to be concentrated under reduced pressure into
8~10 ° of Baume degrees；
D), refine；It will obtain that purified water dissolution is added in extracting solution, the trifluoro methylsulphur of mixture quality 4~6% is then added
Acid, after 90~95 DEG C of 20~30min of closed hydrolysis, vacuum recycling trifluoromethanesulfonic acid obtains liquid of extracting polysaccharide at 45~65 DEG C；
E), chromatograph: resin cation is added in liquid of extracting polysaccharide, is washed with purified water, and combination system obtains eluent；
F), purify: eluent first being poured into alumina column adsorption bleaching, then is placed in reaction kettle, 3~5% active powdered carbons are added,
Impregnate 20min after mixing at 50~60 DEG C, and with obtaining notoginseng polysaccharide solution after stud filter refined filtration；
G), be concentrated: notoginseng polysaccharide solution is first concentrated under reduced pressure into 15~20 ° of Baume degrees, pours into n-butanol after stirring and stands, and is layered
After separate n-butanol layer, be concentrated under reduced pressure into 20~25 ° of Baume degrees, be made notoginseng polysaccharide crystalline deposit object；
H), dry: purified water being added in sediment, adjusts density, by vacuum drying 2~3 hours, notoginseng polysaccharide is made.
2. the extracting method of notoginseng polysaccharide according to claim 1, which is characterized in that in the step A, the ethyl alcohol of addition
Solution quality is 8~12 times of Radix Notoginseng quality.
3. the extracting method of notoginseng polysaccharide according to claim 1, which is characterized in that the filter core mistake of the stud filter
0.25~0.4 micron of precision of filter.
4. the extracting method of notoginseng polysaccharide according to claim 1, which is characterized in that in the step E, resin cation
It is 3~4:1 with liquid of extracting polysaccharide mass ratio, when being washed with purified water, the volume ratio of purified water and resin cation is 9:
1, the flow velocity for being passed through purified water is 300~350L/h.
5. the extracting method of notoginseng polysaccharide according to claim 1, which is characterized in that in the step H, in sediment
It is 1.02~1.15 that purified water adjustment density, which is added, and drying temperature is not less than 85 DEG C, and vacuum degree is not less than -0.1mpa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533818A (en) * | 2020-04-03 | 2020-08-14 | 浙江万里学院 | Decolorizing method for sargassum fusiforme polysaccharide |
| CN114031694A (en) * | 2021-12-23 | 2022-02-11 | 云南三七科技有限公司 | Extraction method of pseudo-ginseng polysaccharide |
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| US20140243517A1 (en) * | 2003-01-03 | 2014-08-28 | Astrazeneca Ab | Methods of producing c-aryl glucoside sglt2 inhibitors |
| CN106749731A (en) * | 2016-12-21 | 2017-05-31 | 云南三七科技有限公司 | A kind of preparation method and application of small molecule notoginseng polysaccharide extract |
| CN106832037A (en) * | 2017-03-30 | 2017-06-13 | 云南润嘉药业有限公司 | A kind of notoginseng polysaccharide extracting method rapidly and efficiently |
| CN107082821A (en) * | 2017-05-02 | 2017-08-22 | 江苏大学 | A kind of method for purifying plant polyose |
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2019
- 2019-05-27 CN CN201910443332.XA patent/CN110105459A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140243517A1 (en) * | 2003-01-03 | 2014-08-28 | Astrazeneca Ab | Methods of producing c-aryl glucoside sglt2 inhibitors |
| CN106749731A (en) * | 2016-12-21 | 2017-05-31 | 云南三七科技有限公司 | A kind of preparation method and application of small molecule notoginseng polysaccharide extract |
| CN106832037A (en) * | 2017-03-30 | 2017-06-13 | 云南润嘉药业有限公司 | A kind of notoginseng polysaccharide extracting method rapidly and efficiently |
| CN107082821A (en) * | 2017-05-02 | 2017-08-22 | 江苏大学 | A kind of method for purifying plant polyose |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533818A (en) * | 2020-04-03 | 2020-08-14 | 浙江万里学院 | Decolorizing method for sargassum fusiforme polysaccharide |
| CN114031694A (en) * | 2021-12-23 | 2022-02-11 | 云南三七科技有限公司 | Extraction method of pseudo-ginseng polysaccharide |
| CN114031694B (en) * | 2021-12-23 | 2023-02-03 | 云南三七科技有限公司 | Extraction method of pseudo-ginseng polysaccharide |
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