CN105777922A - Pilose asiabell root polysaccharide extraction method - Google Patents
Pilose asiabell root polysaccharide extraction method Download PDFInfo
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- CN105777922A CN105777922A CN201410834418.2A CN201410834418A CN105777922A CN 105777922 A CN105777922 A CN 105777922A CN 201410834418 A CN201410834418 A CN 201410834418A CN 105777922 A CN105777922 A CN 105777922A
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- radix codonopsis
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Abstract
The invention provides a pilose asiabell root polysaccharide extraction method. The method is characterized in comprising the following steps: pilose asiabell root is dried and pulverized to a size of 40-100 meshes; the pilose asiabell root powder is subjected to reflux extraction with a chloroform/methanol mixed solvent; a filter cake obtained by filtering is subjected to alcohol extraction, and is then subjected to leaching with water; filtration is carried out, and a filtrate is concentrated; the concentrate liquid is subjected to alcohol precipitation; filtration is carried out, and pilose asiabell root crude polysaccharide is obtained; the pilose asiabell root crude polysaccharide is treated in an n-butanol/trichloroacetic acid mixed solvent; the obtained material is dissolved in water and is loaded in a chromatography column; elution is carried out; the effluent is subjected to concentration, alcohol precipitation, filtration and drying, such that pilose asiabell root polysaccharide is obtained. The pilose asiabell root polysaccharide extraction method provided by the invention is simple, and a deproteinization effect is good. The extracted pilose asiabell root polysaccharide has the advantages of low impurity content, high yield and high purity.
Description
Technical field
The present invention relates to the extracting method of active ingredients from traditional Chinese medicinal, specifically the extracting method of Radix Codonopsis polysaccharide.
Background technology
Radix Codonopsis (RootofPiloseAsiabell) is campanulaceae Codonopsis plant, is used as medicine with dry root, can invigorating the spleen and replenishing QI, spleen invigorating lung benefiting, for deficiency of the spleen and lung, cardiopalmus of breathing hard, anorexia and loose stool, dyspnea due to deficiency cough, interior-heat disappears and coughs.Radix Codonopsis, mainly containing various saccharides, phenols, sterol, volatile oil, scutellarein glucosid, Saponin and Alkaloid and nitrogen containing component, has enhancing immunity, expansion blood vessel, blood pressure lowering, improves microcirculation, strengthens the effects such as hemopoietic function.
Radix Codonopsis polysaccharide has the good biological activity of many aspects, and modern pharmacological research shows, Radix Codonopsis polysaccharide has the effects such as adjustment immunity of organisms, defying age, anti-hypoxia, anti-stress, antioxidation, can be widely applied to medicine, food industry.
At present, Radix Codonopsis polysaccharide extractive technique mainly has water lift-off centrifugal separation, decoction and alcohol sedimentation technique etc., but existing extracting method selects unreasonable due to technical parameter, processing step is more complicated, extract the Radix Codonopsis polysaccharide impurities obtained more, Deproteinization weak effect, and the productivity of the Radix Codonopsis polysaccharide obtained and purity are all relatively low, are unfavorable for production application.
Summary of the invention
It is an object of the invention to avoid prior art defect, it is provided that a kind of technique is simple, and Deproteinization effect is good, extract the Radix Codonopsis polysaccharide impurities obtained few, the extracting method of productivity and the high Radix Codonopsis polysaccharide of purity.
The present invention adopts following technical scheme to realize:
The extracting method of a kind of Radix Codonopsis polysaccharide, it is characterised in that comprise the following steps:
(1) pretreatment: choose after Radix Codonopsis root carries out washing, removes impurity, dried, pulverize, cross 40-100 mesh sieve, obtain Radix Codonopsis powder；
(2) degreasing decoloring: joined in chloroform/methanol mixed solvent by Radix Codonopsis powder obtained above, be warming up to backflow, carries out degreasing decoloring process, filters, collects filter cake；
(3) extract: the filter cake obtained in step (2) is joined in alcoholic solvent, it is warming up to backflow, back flow reaction 2-6h, filters, is then added in water by the solids obtained, it is warming up to 50-70 DEG C, stirring, extracts 0.5-2h, filters, collecting filtrate, remaining residue can extract again；
(4) concentrate drying: the filtrate obtained in step (3) is warming up to 60-80 DEG C, carries out concentrating under reduced pressure, obtain concentrated solution, the concentrated solution of gained is mixed with alcoholic solution, carries out precipitate with ethanol process, filter, wash with organic solvent, obtain Radix Codonopsis crude polysaccharides；
(5) purification is separated: joined by Radix Codonopsis crude polysaccharides after n-butyl alcohol/ethapon mixed solvent carries out deproteinization process, with joining in chromatographic column after aqueous solvent, eluting is carried out again with the sodium chloride solution of 0.05mol/L-0.15mol/L, collect effluent, concentrating under reduced pressure, precipitate with ethanol, filtration, dry, obtain Radix Codonopsis polysaccharide.
The extracting method of described Radix Codonopsis polysaccharide, in step (2), chloroform/methanol mixed solvent is 5-15:1 with the weight ratio of Radix Codonopsis powder；The chloroform of chloroform/methanol mixed solvent and the volume ratio of methanol are 3:1.
The extracting method of described Radix Codonopsis polysaccharide, in step (3), alcoholic solvent is 75%-85% ethanol water.
The extracting method of described Radix Codonopsis polysaccharide, in step (3), remaining residue can extract again, is added to the water by remaining residue, is warming up to 50-70 DEG C, stirring, extracts 0.5-2h, filters, and collects filtrate, and remaining residue can extract again；Repeat to extract 2-3 time, merge the filtrate collected.
The extracting method of described a kind of Radix Codonopsis polysaccharide, what the precipitate with ethanol described in step (4) processed concretely comprises the following steps: the volume ratio adding the alcoholic solution of 90%-100%, alcoholic solution and concentrated solution in the concentrated solution of gained is 3-8:1；Stirring 10-30min, after low temperature (-5-10 DEG C) stands 10-15h, filters, obtains Radix Codonopsis crude polysaccharides.
The extracting method of described a kind of Radix Codonopsis polysaccharide, it is 0.5-1.5:1 that n-butyl alcohol/tri-described in step (5) filter the weight ratio of acetic acid solvent and Radix Codonopsis crude polysaccharides；Wherein in n-butyl alcohol/trichloroacetic acid mixed solvent, the volume ratio of n-butyl alcohol and trichloroacetic acid is 10-30:1.
The extracting method of described a kind of Radix Codonopsis polysaccharide, the described chromatographic column in step (5) is sephadex column.
The extracting method of described a kind of Radix Codonopsis polysaccharide, the elution speed described in step (5) is 0.5mL/min-1.5mL/min.
Beneficial effects of the present invention: the extracting method of a kind of Radix Codonopsis polysaccharide of the present invention, Deproteinization effect is good, and degreasing decoloring is effective, and the Radix Codonopsis polysaccharide productivity obtained and purity are high；Equipment required for the present invention is the equipment that this area is common, and technique is simple, with low cost, have higher economic well-being of workers and staff.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention done concrete introduction.
Embodiment 1
Choose Radix Codonopsis root first to wash, after rejecting impurity, dry when 60 DEG C, then pulverizer is adopted to carry out being crushed to 50 orders, obtain Radix Codonopsis powder, weigh 100g Radix Codonopsis powder and add 500g chloroform/methanol mixed solvent, when being warming up to 60 DEG C, backflow 2h, carry out degreasing decoloring process, after backflow terminates, filter, remove filtrate, collect filter cake, the filter cake of collection is joined in the ethanol water of 80%, it is warming up to backflow 2h when 80 DEG C, after backflow terminates, filter, remove filtrate, the solids obtained is joined in 100ml distilled water, it is warming up to 60 DEG C, 1h is extracted in stirring, filter, collect filtrate, remaining residue can extract again；When the filtrate of collection is warming up to 60-70 DEG C, carry out decompression distillation and concentration, it is concentrated into about 30ml concentrated solution, concentrated solution adds the ethanol water of 180ml95%, stirring, is cooled to 0 DEG C, is stirred for 30min, then after low temperature (-5-10 DEG C) stands 12h, after standing terminates, adopting centrifuge to be centrifuged, rotating speed is 2000r/min, wash with dehydrated alcohol, acetone successively after centrifugal, after centrifuge dripping, put in vacuum drier, control temperature at 50-55 DEG C, dry 5h, obtains Radix Codonopsis crude polysaccharides.
nullAbove-mentioned Radix Codonopsis crude polysaccharides is added in n-butyl alcohol/trichloroacetic acid mixed solvent，Weight ratio is 1:1，Wherein in n-butyl alcohol/trichloroacetic acid mixed solvent, both volume ratios are 20:1，Then heat under 60 DEG C of conditions，Backflow 2h，After carrying out deproteinization process，Some small molecular weight impurities are removed again through dialysis，Then the Radix Codonopsis crude polysaccharides obtained is joined after distilled water making be completely dissolved，It is then added in sephadex column，Eluting is carried out with the sodium chloride solution of 0.1mol/L，Elution speed is 1mL/min，Collect effluent，Then the effluent obtained is joined in other reaction vessel，Heating，It is warming up to 50-55 DEG C，Concentrating under reduced pressure，It is concentrated into the 1/5 of former effluent volume，Obtain concentrated solution，Add in concentrated solution again its volume 5 times amount 95% ethanol water，Under stirring，It is cooled to 0 DEG C，Continue stirring 30min，Then 12h is stood，After standing terminates，Employing centrifuge is centrifuged，Rotating speed is 2000r/min，Dehydrated alcohol is used again successively after centrifugal、Acetone washs，After centrifuge dripping，The Radix Codonopsis polysaccharide obtained is put in vacuum drier，Control temperature at 50-55 DEG C，Radix Codonopsis polysaccharide finished product is obtained after dry 8h.
Embodiment 2
Choose Radix Codonopsis root first to wash, after rejecting impurity, dry when 60 DEG C, then pulverizer is adopted to carry out being crushed to 70 orders, obtain Radix Codonopsis powder, weigh 100g Radix Codonopsis powder and add 1000g chloroform/methanol mixed solvent, when being warming up to 60 DEG C, backflow 2h, carry out degreasing decoloring process, after backflow terminates, filter, remove filtrate, collect filter cake, the filter cake of collection is joined in the ethanol water of 85%, it is warming up to backflow 2h when 80 DEG C, after backflow terminates, filter, remove filtrate, the solids obtained is joined in 100ml distilled water, it is warming up to 60 DEG C, 1h is extracted in stirring, filter, collect filtrate, remaining residue can extract again；When the filtrate of collection is warming up to 60-70 DEG C, carry out decompression distillation and concentration, it is concentrated into about 30ml concentrated solution, concentrated solution adds the ethanol water of 200ml95%, stirring, is cooled to 0 DEG C, is stirred for 30min, then after low temperature (-5-10 DEG C) stands 12h, after standing terminates, adopting centrifuge to be centrifuged, rotating speed is 2000r/min, wash with dehydrated alcohol, acetone successively after centrifugal, after centrifuge dripping, put in vacuum drier, control temperature at 50-55 DEG C, dry 5h, obtains Radix Codonopsis crude polysaccharides.
nullAbove-mentioned Radix Codonopsis crude polysaccharides is added in n-butyl alcohol/trichloroacetic acid mixed solvent，Weight ratio is 1:1.2，Wherein in n-butyl alcohol/trichloroacetic acid mixed solvent, both volume ratios are 20:1，Then heat under 60 DEG C of conditions，Backflow 2h，After carrying out deproteinization process，Some small molecular weight impurities are removed again through dialysis，Then the Radix Codonopsis crude polysaccharides obtained is joined after distilled water making be completely dissolved，It is then added in sephadex column，Eluting is carried out with the sodium chloride solution of 0.1mol/L，Elution speed is 1ml/min，Collect effluent，Then the effluent obtained is joined in other reaction vessel，Heating，It is warming up to 50-55 DEG C，Concentrating under reduced pressure，It is concentrated into the 1/5 of former effluent volume，Obtain concentrated solution，Add in concentrated solution again its volume 5 times amount 95% ethanol water，Under stirring，It is cooled to 0 DEG C，Continue stirring 30min，Then 12h is stood，After standing terminates，Employing centrifuge is centrifuged，Rotating speed is 2000r/min，Dehydrated alcohol is used again successively after centrifugal、Acetone washs，After centrifuge dripping，The Radix Codonopsis polysaccharide obtained is put in vacuum drier，Control temperature at 50-55 DEG C，Radix Codonopsis polysaccharide finished product is obtained after dry 8h.
Specific embodiment described in the present invention is only to present invention explanation for example, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement etc., all fall within protection scope of the present invention.
Claims (8)
1. the extracting method of a Radix Codonopsis polysaccharide, it is characterised in that comprise the following steps:
(1) pretreatment: choose after Radix Codonopsis root carries out washing, removes impurity, dried, pulverize, cross 40-100 mesh sieve, obtain Radix Codonopsis powder；
(2) degreasing decoloring: joined in chloroform/methanol mixed solvent by Radix Codonopsis powder obtained above, be warming up to backflow, carries out degreasing decoloring process, filters, collects filter cake；
(3) extract: the filter cake obtained in step (2) is joined in alcoholic solvent, it is warming up to backflow, back flow reaction 2-6h, filters, is then added in water by the solids obtained, it is warming up to 50-70 DEG C, stirring, extracts 0.5-2h, filters, collecting filtrate, remaining residue can extract again；
(4) concentrate drying: the filtrate obtained in step (3) is warming up to 60-80 DEG C, carries out concentrating under reduced pressure, obtain concentrated solution, the concentrated solution of gained is mixed with alcoholic solution, carries out precipitate with ethanol process, filter, wash with organic solvent, obtain Radix Codonopsis crude polysaccharides；
(5) purification is separated: joined by Radix Codonopsis crude polysaccharides after n-butyl alcohol/ethapon mixed solvent carries out deproteinization process, with joining in chromatographic column after aqueous solvent, eluting is carried out again with the sodium chloride solution of 0.05mol/L-0.15mol/L, collect effluent, concentrating under reduced pressure, precipitate with ethanol, filtration, dry, obtain Radix Codonopsis polysaccharide.
2. the extracting method of a kind of Radix Codonopsis polysaccharide according to claim 1, it is characterised in that: the weight ratio of the chloroform/methanol mixed solvent described in step (2) and Radix Codonopsis powder is 5-15:1；The chloroform of described chloroform/methanol mixed solvent and the volume ratio of methanol are 3:1.
3. the extracting method of a kind of Radix Codonopsis polysaccharide according to claim 1, it is characterised in that: the alcoholic solvent described in step (3) is 75%-85% ethanol water.
4. the extracting method of a kind of Radix Codonopsis polysaccharide according to claim 1, it is characterized in that: the remaining residue described in step (3) can extract again, concrete process is: be added to the water by remaining residue, it is warming up to 50-70 DEG C, stirring, extracts 0.5-2h, filters, collecting filtrate, remaining residue can extract again；Repeat to extract 2-3 time, merge and collect filtrate.
5. the extracting method of a kind of Radix Codonopsis polysaccharide according to claim 1, it is characterized in that: what the precipitate with ethanol described in step (4) processed concretely comprises the following steps: the volume ratio adding the alcoholic solution of 90%-100%, described alcoholic solution and concentrated solution in the concentrated solution of gained is 3-8:1；Stirring 10-30min, after stand at low temperature 10-15h, filters, obtains Radix Codonopsis crude polysaccharides.
6. the extracting method of a kind of Radix Codonopsis polysaccharide according to claim 1, it is characterised in that: it is 0.5-1.5:1 that n-butyl alcohol/tri-described in step (5) filter the weight ratio of acetic acid solvent and Radix Codonopsis crude polysaccharides；In described n-butyl alcohol/trichloroacetic acid mixed solvent, n-butyl alcohol is 10-30:1 with the volume ratio of trichloroacetic acid.
7. the extracting method of a kind of Radix Codonopsis polysaccharide according to claim 1, it is characterised in that: the described chromatographic column in step (5) is sephadex column.
8. the extracting method of a kind of Radix Codonopsis polysaccharide according to claim 1, it is characterised in that: the elution speed described in step (5) is 0.5mL/min-1.5mL/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410834418.2A CN105777922A (en) | 2014-12-26 | 2014-12-26 | Pilose asiabell root polysaccharide extraction method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266688A (en) * | 2018-09-25 | 2019-01-25 | 武汉轻工大学 | A kind of preparation method and applications of Codonopsis pilosula polysaccharide |
| CN115677868A (en) * | 2022-08-23 | 2023-02-03 | 重庆市中药研究院 | Extraction method of total polysaccharides of eggplanthus altissima |
-
2014
- 2014-12-26 CN CN201410834418.2A patent/CN105777922A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266688A (en) * | 2018-09-25 | 2019-01-25 | 武汉轻工大学 | A kind of preparation method and applications of Codonopsis pilosula polysaccharide |
| CN115677868A (en) * | 2022-08-23 | 2023-02-03 | 重庆市中药研究院 | Extraction method of total polysaccharides of eggplanthus altissima |
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