CN103709263A - Purification method of natural polysaccharides - Google Patents
Purification method of natural polysaccharides Download PDFInfo
- Publication number
- CN103709263A CN103709263A CN201310656927.6A CN201310656927A CN103709263A CN 103709263 A CN103709263 A CN 103709263A CN 201310656927 A CN201310656927 A CN 201310656927A CN 103709263 A CN103709263 A CN 103709263A
- Authority
- CN
- China
- Prior art keywords
- macroporous
- natural polysaccharide
- chromatography column
- exchange resin
- ion exchange
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a purification method of natural polysaccharides. The invention solves the problem of the prior art that single usage of macroporous weak basic anion exchange resin for purification of polysaccharides can't effectively remove pigment, inorganic salt and polyphenol in the natural polysaccharides. The invention uses a combination of macroporous weak basic anion exchange resin and macroporous resin, and effectively solves the above problem through the removal of organic pigments, inorganic salt, polyphenols and other impurities in the polysaccharides.
Description
Technical field
The present invention relates to a kind of purification process, more particularly, the present invention relates to a kind of purification process of natural polysaccharide.
Background technology
The polysaccharide material extracting from multiple natural product is because it can effectively improve the concern that human immunological competence is subject to people.But in the extraction preparation process of natural polysaccharide compound, owing to containing the impurity such as multiple organic pigment, inorganic salt, polyphenol substance in raw material, make natural polysaccharide compound in use have the shortcomings such as color is excessively dark, package stability is poor, the certain side effect of tool, bring serious problems to production and the effect of polysaccharide.
It is CN101050241 that State Intellectual Property Office discloses a publication number in 2007.10.10, and name is called the patent of invention of " preparation method of MDG-1 polysaccharide of lilyturf root-1 ", and this patent relates to a kind of preparation method with MDG-1 polysaccharide of lilyturf root-1 of function of resisting myocardial ischemia.First this preparation method obtains the Crude polysaccharides tuber of dwarf lilyturf by Tubers of Ophiopogon japonicus after water extract-alcohol precipitation is dry, the tuber of dwarf lilyturf, Crude polysaccharides adopted hyperfiltration process separated, again the concentrated solution after ultrafiltration is carried out to wash-out with macropore weak basic anion exchange resin with water, collect the wash-out part of 4-8 times of column volume, after merging, dry, obtain MDG-1 polysaccharide of lilyturf root-1, its purity >=90%.Adopt the inventive method to prepare MDG-1 polysaccharide of lilyturf root-1, consuming time short, cost is low, can prepare in a large number and adapt to suitability for industrialized production.
The preparation method of MDG-1 polysaccharide of lilyturf root-1 in above-mentioned patent has adopted macropore weak basic anion exchange resin, but still has the problem that can not disposablely effectively remove the impurity such as pigment, inorganic salt and polyphenol in natural polysaccharide.
Summary of the invention
The present invention is intended to solve the macropore weak basic anion exchange resin that only adopts of the prior art polysaccharide is carried out to purifying, can not disposablely effectively remove the problem of the impurity such as pigment, inorganic salt and polyphenol in natural polysaccharide, a kind of purification process of natural polysaccharide is provided, can disposablely effectively removes the impurity such as pigment, inorganic salt and polyphenol in natural polysaccharide.
To achieve these goals, concrete technical scheme of the present invention is as follows:
A purification process for natural polysaccharide, is characterized in that: comprise following processing step:
A, adopt 1N HCl and 1N NaOH to carry out alternate treatment macroporous weak base ion exchange resin;
B, the macroporous weak base ion exchange resin of processing is transferred in chromatography column and continues to process with 1N NaOH;
C, with deionized water, clean the NaOH in macroporous weak base ion exchange resin in chromatography column, standby;
D, macroporous adsorbent resin is filled in chromatography column, then adopt alcohol to process;
E, with deionized water, wash away the alcohol in macroporous adsorbent resin in chromatography column, standby;
F, with the flow velocity of 10ml/h, make natural polysaccharide extracting solution by macroporous weak base ion exchange resin chromatography column and the macroporous adsorption resin chromatography post of series connection;
The natural polysaccharide extracting solution product that G, collection are flowed out;
H, concentrate drying obtain the natural polysaccharide product after purifying.
The consumption volume ratio of natural polysaccharide extracting solution of the present invention, macroporous weak base ion exchange resin, macroporous adsorbent resin, 1N HCl, 1N NaOH, alcohol and deionized water is 1:0.1:0.1:3:3:5:5.
The present invention obtains after the natural polysaccharide product after purifying at described concentrate drying, with deionized water, wash away natural polysaccharide extracting solution residual in chromatography column, pigment with the absorption of 1N NaOH wash-out macroporous weak base ion exchange resin, with deionized water, wash away the NaOH in chromatography column again, macroporous weak base ion exchange resin chromatography column after regeneration is for next cycle, and the impurity that employing alcohol washes away absorption with macroporous adsorbent resin is for next cycle.
Macroporous weak base ion exchange resin of the present invention and macroporous adsorbent resin are that polysaccharide extracts conventional resin in purifying.
The useful technique effect that the present invention brings:
The invention solves the macropore weak basic anion exchange resin that only adopts of the prior art polysaccharide is carried out to purifying, can not disposablely effectively remove the problem of the impurity such as pigment, inorganic salt and polyphenol in natural polysaccharide, select the combination of macroporous weak base ion exchange resin-macroporous adsorbent resin, by impurity such as the organic pigment in Polysaccharide removing, inorganic salt, polyphenol substances, efficiently solved such problem.Adopt the impurity such as pigment, inorganic salt and polyphenol of macroporous weak base ion exchange resin resin-macroporous adsorption resin chromatography method in can disposable effective removal natural polysaccharide, there is the advantages such as simple to operate, cost is low, removal effect is good, polysaccharide product purity is high, product result of use is good.
Embodiment
embodiment 1
A purification process for natural polysaccharide, comprises following processing step:
A, adopt 1N HCl and 1N NaOH to carry out alternate treatment macroporous weak base ion exchange resin;
B, the macroporous weak base ion exchange resin of processing is transferred in chromatography column and continues to process with 1N NaOH;
C, with deionized water, clean the NaOH in macroporous weak base ion exchange resin in chromatography column, standby;
D, macroporous adsorbent resin is filled in chromatography column, then adopt alcohol to process;
E, with deionized water, wash away the alcohol in macroporous adsorbent resin in chromatography column, standby;
F, with the flow velocity of 10ml/h, make natural polysaccharide extracting solution by macroporous weak base ion exchange resin chromatography column and the macroporous adsorption resin chromatography post of series connection;
The natural polysaccharide extracting solution product that G, collection are flowed out;
H, concentrate drying obtain the natural polysaccharide product after purifying.
embodiment 2
A purification process for natural polysaccharide, comprises following processing step:
A, adopt 1N HCl and 1N NaOH to carry out alternate treatment macroporous weak base ion exchange resin;
B, the macroporous weak base ion exchange resin of processing is transferred in chromatography column and continues to process with 1N NaOH;
C, with deionized water, clean the NaOH in macroporous weak base ion exchange resin in chromatography column, standby;
D, macroporous adsorbent resin is filled in chromatography column, then adopt alcohol to process;
E, with deionized water, wash away the alcohol in macroporous adsorbent resin in chromatography column, standby;
F, with the flow velocity of 10ml/h, make natural polysaccharide extracting solution by macroporous weak base ion exchange resin chromatography column and the macroporous adsorption resin chromatography post of series connection;
The natural polysaccharide extracting solution product that G, collection are flowed out;
H, concentrate drying obtain the natural polysaccharide product after purifying.
The consumption volume ratio of described natural polysaccharide extracting solution, macroporous weak base ion exchange resin, macroporous adsorbent resin, 1N HCl, 1N NaOH, alcohol and deionized water is 1:0.1:0.1:3:3:5:5.
embodiment 3
A purification process for natural polysaccharide, comprises following processing step:
A, adopt 1N HCl and 1N NaOH to carry out alternate treatment macroporous weak base ion exchange resin;
B, the macroporous weak base ion exchange resin of processing is transferred in chromatography column and continues to process with 1N NaOH;
C, with deionized water, clean the NaOH in macroporous weak base ion exchange resin in chromatography column, standby;
D, macroporous adsorbent resin is filled in chromatography column, then adopt alcohol to process;
E, with deionized water, wash away the alcohol in macroporous adsorbent resin in chromatography column, standby;
F, with the flow velocity of 10ml/h, make natural polysaccharide extracting solution by macroporous weak base ion exchange resin chromatography column and the macroporous adsorption resin chromatography post of series connection;
The natural polysaccharide extracting solution product that G, collection are flowed out;
H, concentrate drying obtain the natural polysaccharide product after purifying.
At described concentrate drying, obtain after the natural polysaccharide product after purifying, with deionized water, wash away natural polysaccharide extracting solution residual in chromatography column, pigment with the absorption of 1N NaOH wash-out macroporous weak base ion exchange resin, with deionized water, wash away the NaOH in chromatography column again, macroporous weak base ion exchange resin chromatography column after regeneration is for next cycle, and the impurity that employing alcohol washes away absorption with macroporous adsorbent resin is for next cycle.
Claims (3)
1. a purification process for natural polysaccharide, is characterized in that: comprise following processing step:
A, adopt 1N HCl and 1N NaOH to carry out alternate treatment macroporous weak base ion exchange resin;
B, the macroporous weak base ion exchange resin of processing is transferred in chromatography column and continues to process with 1N NaOH;
C, with deionized water, clean the NaOH in macroporous weak base ion exchange resin in chromatography column, standby;
D, macroporous adsorbent resin is filled in chromatography column, then adopt alcohol to process;
E, with deionized water, wash away the alcohol in macroporous adsorbent resin in chromatography column, standby;
F, with the flow velocity of 10ml/h, make natural polysaccharide extracting solution by macroporous weak base ion exchange resin chromatography column and the macroporous adsorption resin chromatography post of series connection;
The natural polysaccharide extracting solution product that G, collection are flowed out;
H, concentrate drying obtain the natural polysaccharide product after purifying.
2. the purification process of a kind of natural polysaccharide according to claim 1, is characterized in that: the consumption volume ratio of described natural polysaccharide extracting solution, macroporous weak base ion exchange resin, macroporous adsorbent resin, 1N HCl, 1N NaOH, alcohol and deionized water is 1:0.1:0.1:3:3:5:5.
3. the purification process of a kind of natural polysaccharide according to claim 1, it is characterized in that: at described concentrate drying, obtain after the natural polysaccharide product after purifying, with deionized water, wash away natural polysaccharide extracting solution residual in chromatography column, pigment with the absorption of 1N NaOH wash-out macroporous weak base ion exchange resin, with deionized water, wash away the NaOH in chromatography column again, macroporous weak base ion exchange resin chromatography column after regeneration is for next cycle, and the impurity that employing alcohol washes away absorption with macroporous adsorbent resin is for next cycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310656927.6A CN103709263A (en) | 2013-12-09 | 2013-12-09 | Purification method of natural polysaccharides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310656927.6A CN103709263A (en) | 2013-12-09 | 2013-12-09 | Purification method of natural polysaccharides |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103709263A true CN103709263A (en) | 2014-04-09 |
Family
ID=50402647
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310656927.6A Pending CN103709263A (en) | 2013-12-09 | 2013-12-09 | Purification method of natural polysaccharides |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103709263A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589151A (en) * | 2016-12-09 | 2017-04-26 | 彭雅龙 | Ion exchange chromatogram purification preparation method of garlic polysaccharide |
| CN106754770A (en) * | 2016-12-05 | 2017-05-31 | 璧典匠 | A kind of chromatographic purifying preparation method of superoxide dismutase |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683418A (en) * | 2005-03-07 | 2005-10-19 | 敖宗华 | Process for preparing antrodia camphorata polysaccharide and antrodia camphorata triterpene with micro-prorous adsorptive resin and its product |
| JP2012121784A (en) * | 2010-12-08 | 2012-06-28 | Shanghai Huayi Microelectric Material Co Ltd | Method and device for refining aqueous hydrogen peroxide solution |
| CN102648750A (en) * | 2012-05-07 | 2012-08-29 | 南京中医药大学 | Refine Chinese date cane sugar, Chinese date high fructose syrup and preparation method of refine Chinese date cane sugar and Chinese date high fructose syrup |
| CN102786566A (en) * | 2012-09-07 | 2012-11-21 | 谱赛科（江西）生物技术有限公司 | Method for absorbing and purifying stevioside through multiple-column secondary resin series connection |
| CN102816193A (en) * | 2012-09-13 | 2012-12-12 | 江南大学 | Method for extracting and purifying steviol glycoside from stevia rebaudiana aqueous extract by virtue of series resin column method |
| CN103030708A (en) * | 2012-12-13 | 2013-04-10 | 大兴安岭林格贝有机食品有限责任公司 | Novel purification method of lycium chinense polysaccharide |
| CN103169761A (en) * | 2013-04-10 | 2013-06-26 | 广州中医药大学 | Effective part of traditional Chinese medicine compound Chinese angelica blood replenishing soup and synchronous preparation method and application thereof |
| CN103204839A (en) * | 2013-03-29 | 2013-07-17 | 亿利资源集团有限公司 | Synchronous preparation method of effective ingredient of licorice |
-
2013
- 2013-12-09 CN CN201310656927.6A patent/CN103709263A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683418A (en) * | 2005-03-07 | 2005-10-19 | 敖宗华 | Process for preparing antrodia camphorata polysaccharide and antrodia camphorata triterpene with micro-prorous adsorptive resin and its product |
| JP2012121784A (en) * | 2010-12-08 | 2012-06-28 | Shanghai Huayi Microelectric Material Co Ltd | Method and device for refining aqueous hydrogen peroxide solution |
| CN102648750A (en) * | 2012-05-07 | 2012-08-29 | 南京中医药大学 | Refine Chinese date cane sugar, Chinese date high fructose syrup and preparation method of refine Chinese date cane sugar and Chinese date high fructose syrup |
| CN102786566A (en) * | 2012-09-07 | 2012-11-21 | 谱赛科（江西）生物技术有限公司 | Method for absorbing and purifying stevioside through multiple-column secondary resin series connection |
| CN102816193A (en) * | 2012-09-13 | 2012-12-12 | 江南大学 | Method for extracting and purifying steviol glycoside from stevia rebaudiana aqueous extract by virtue of series resin column method |
| CN103030708A (en) * | 2012-12-13 | 2013-04-10 | 大兴安岭林格贝有机食品有限责任公司 | Novel purification method of lycium chinense polysaccharide |
| CN103204839A (en) * | 2013-03-29 | 2013-07-17 | 亿利资源集团有限公司 | Synchronous preparation method of effective ingredient of licorice |
| CN103169761A (en) * | 2013-04-10 | 2013-06-26 | 广州中医药大学 | Effective part of traditional Chinese medicine compound Chinese angelica blood replenishing soup and synchronous preparation method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 史作清等: "《吸附分离树脂在医药工业中的应用》", 30 September 2008, 化学工业出版社 * |
| 邱立友: "《发酵工程与设备（第1版）》", 31 August 2007, 中国农业出版社 * |
| 陈晓青等: "《中草药成分分离分析技术与方法（第1版）》", 30 April 2006, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106754770A (en) * | 2016-12-05 | 2017-05-31 | 璧典匠 | A kind of chromatographic purifying preparation method of superoxide dismutase |
| CN106589151A (en) * | 2016-12-09 | 2017-04-26 | 彭雅龙 | Ion exchange chromatogram purification preparation method of garlic polysaccharide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102816193B (en) | A kind of method of resin column method extraction purification steviol glycoside from stevia rebaudiana water extract of connecting | |
| CN103467540B (en) | A kind of method extracting rhodioside from Root of Kirilow Rhodiola | |
| CN101392011B (en) | Isolation and purification method of natural salidroside | |
| CN101973871B (en) | Electronic grade citric acid and production method thereof | |
| CN102993329B (en) | Method for comprehensively extracting saponin, polysaccharides and polyphenol from camellia oleifera abel defatted cakes | |
| CN102942550B (en) | Method for extracting cyanidin from black bean peel | |
| CN102417194A (en) | Method for deeply removing magnesium through chelating resin for extracting lithium from salt lake brine | |
| CN104177280A (en) | Production process of methionine | |
| CN105037488A (en) | Purification method of melanotan II | |
| CN101935278A (en) | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae | |
| CN106629788B (en) | A kind of production technology of lithium chloride | |
| CN102351926B (en) | A kind of preparation method of arctinin | |
| CN103012544B (en) | A kind of method extracting saponin and polysaccharide from tea seed grouts | |
| CN105315704A (en) | Method for recovering organic acid from waste liquid produced after pigment is extracted from roselle | |
| CN102093441A (en) | After-treatment method for synthesizing neohesperidin dihydrochalcone from neohesperidin | |
| CN103709263A (en) | Purification method of natural polysaccharides | |
| CN101558803A (en) | Extracting and purifying method of extract of bitter leaves | |
| CN106279197B (en) | The purifying of isobide reaction solution and crystallization processes | |
| CN102702286A (en) | Method for separating and purifying aucubin from leaves of eucommia ulmoides oliv with NKA-2 macroporous adsorption resin | |
| CN101987856B (en) | Preparation method of anthocyanin monomer cornflower-3-glucoside | |
| CN102204950B (en) | Method for extracting flavonoid from liquorice waste residue | |
| CN105111144A (en) | Method of extracting nuciferine from lotus leaves | |
| CN104478720A (en) | Method for purifying chlorogenic acid from folium cortex eucommiae extracting solution | |
| CN103058882B (en) | Method for separating natural theanine | |
| CN103965156A (en) | Column chromatography for purification of natural vitamin E |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140409 |
|
| RJ01 | Rejection of invention patent application after publication |