CN1112368C - Water soluble chitosan separating and purifying method - Google Patents
Water soluble chitosan separating and purifying method Download PDFInfo
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- CN1112368C CN1112368C CN00114504A CN00114504A CN1112368C CN 1112368 C CN1112368 C CN 1112368C CN 00114504 A CN00114504 A CN 00114504A CN 00114504 A CN00114504 A CN 00114504A CN 1112368 C CN1112368 C CN 1112368C
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- soluble chitosan
- chitosan
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Abstract
The present invention discloses a method for separating and purifying water soluble chitosan and derivatives thereof. Various kinds of graded chitosan with different molecular weight and different content of carboxyl can be obtained through using strong basic anion-exchange resin (hydroxy type) to separate and purify water soluble chitosan products obtained by a method of the oxidative degradation of hydrogen peroxide. The present invention solves the problem that the existence of side reaction during the process of oxidative degradation makes the separation and the purification difficult, which blocks the application researches of the product.
Description
Technical field
The present invention relates to a kind of the separation and the method for purifying water soluble chitosan, particularly separate method with this type of material of purifying with the oh type strongly basic anion exchange resin.
Background technology
Water-soluble chitosan has many physiologically actives and function, can be prepared by the deacetylation derivative degradation of chitosan of chitin in field widespread uses such as medicine, protective foods, makeup.The water-soluble chitosan that molecular weight varies in size, carboxyl-content is different has many different physiologically actives and function, and its purposes is difference to some extent also, and therefore separation and purifying water soluble chitosan are necessary.In recent years, people are to oxidation degradation method, and especially hydrogen peroxide method research is more, but because the existence of side reaction in the oxidative degradation process separates and purification difficult product, the applied research of product is hindered.
Summary of the invention
The method that the purpose of this invention is to provide a kind of separation and purifying water soluble chitosan, product separates and the difficulty of purifying to solve.
The used solution of the present invention is: chitosan is had carboxyl to generate in the water-soluble products of hydrogen peroxide degradation gained, in general carboxyl is many more in the molecule, and molecular weight is more little.The aqueous solution of water-soluble chitosan product is during through oh type strongly basic anion exchange resin post, do not contain carboxyl or contain carboxyl molecule seldom by deionized water at first wash-out come out.The band carboxyl chitosan molecule that is bonded on the resin can be collected different components successively by the dilute hydrochloric acid wash-out, through concentrating under reduced pressure, collects product, can obtain the water-soluble chitosan product that molecular weight varies in size, carboxyl-content is different.
The 717# resin is used NaOH solution soaking 24 hours, and elimination NaOH solution uses the deionized water wash resin to elutant pH7～8 then.The water-soluble chitosan product of hydrogen peroxide degradation gained is dissolved in the deionized water, be mixed with solution, add chromatographic column top, with hydrochloric acid gradient elution (concentration of hydrochloric acid 0～3 mol), collect different elutriants, concentrating under reduced pressure is collected product, obtains the different chitosan of carboxyl-content or its hydrochloride.
The invention solves because the existence of side reaction in the oxidative degradation process makes product separate and purification difficult the problem that the applied research of product is hindered.With GPC (gel permeation chromatography),
13C NMR (13C nuclear magnetic resonance), IR, the carboxyl-content analysis is analyzed separated product, has proved separating resulting, sees Table 1.
Description of drawings:
Fig. 1: component 1
13C NMR (13C nuclear magnetic resonance) spectrogram
Fig. 2: component 2
13C NMR (13C nuclear magnetic resonance) spectrogram
Fig. 3: component 3
13C NMR (13C nuclear magnetic resonance) spectrogram
Embodiment
Below in conjunction with drawings and the specific embodiments technical solution of the present invention is described further:
Embodiment:
Get 717# resin 100g and pack in the chromatographic column of interior diameter 3cm, with the NaOH solution soaking of 150 milliliter of 4 mol 24 hours, elimination NaOH solution then, with the deionized water wash resin to elutant pH7～8.The water-soluble chitosan product 5g of hydrogen peroxide degradation gained is dissolved in the 20ml deionized water, is mixed with solution, add chromatographic column top, use the deionized water wash-out, elution speed 0.5ml/min, elutant is concentrated, dry, obtains carboxylic hardly chitosan.Use the hydrochloric acid wash-out of 1 mol, 3 mol successively, collect elutriant respectively, concentrating under reduced pressure, washing with alcohol, vacuum-drying obtains containing component 2, the component 3 of carboxyl chitosan hydrochloric acid.Component 1-3's
13C NMR (13C nuclear magnetic resonance) spectrogram such as Fig. 1-3.
Table 1: the analytical results of separated product
M in the table
WThe expression weight-average molecular weight
| Numbering | Yield (%) | IR (1730cm-1) | 13C NMR (160-180ppm) | GPC M W×10-3 | Carboxyl-content (mmol/g) |
| Component 1 | 24.2 | Do not have and absorb | Basic no signal | 5.7 | 0.21 |
| Component 2 | 53.6 | The weak absorption | Weak signal | 4.5 | 1.31 |
| Component 3 | 16.5 | Absorb more by force | Strong signal | 3.4 | 2.32 |
Claims (1)
1. the method for separation and purifying water soluble chitosan, it is characterized in that: the 717# resin was with the NaOH solution soaking of 4 mol 24 hours, elimination NaOH solution then, with the deionized water wash resin to elutant pH7～8, the water-soluble chitosan product of hydrogen peroxide degradation gained is dissolved in the deionized water, be mixed with solution, add chromatographic column top, with concentration is the hydrochloric acid gradient elution of 0～3 mol, collect different elutriants, concentrating under reduced pressure is collected product, obtains molecular weight, different chitosan or its salt of hydroxy radical content.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00114504A CN1112368C (en) | 2000-04-20 | 2000-04-20 | Water soluble chitosan separating and purifying method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00114504A CN1112368C (en) | 2000-04-20 | 2000-04-20 | Water soluble chitosan separating and purifying method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1318568A CN1318568A (en) | 2001-10-24 |
| CN1112368C true CN1112368C (en) | 2003-06-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00114504A Expired - Fee Related CN1112368C (en) | 2000-04-20 | 2000-04-20 | Water soluble chitosan separating and purifying method |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58164601A (en) * | 1982-03-26 | 1983-09-29 | Kohjin Co Ltd | Production of water-soluble chitosan salt |
| JPH0393902A (en) * | 1989-09-05 | 1991-04-18 | Tokai Riyokaku Tetsudo Kk | Ground coil laying method |
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| CN1085564A (en) * | 1993-08-20 | 1994-04-20 | 连云港开发区金祥贸易有限公司 | A kind of preparation method of chitin |
| CN1089620A (en) * | 1993-12-15 | 1994-07-20 | 屈步华 | Preparation method and product with natural structure chitin |
| CN1138336A (en) * | 1994-12-02 | 1996-12-18 | 汉克尔股份两合公司 | Cationic biopolymers |
| JPH115803A (en) * | 1997-06-18 | 1999-01-12 | Tottori Pref Gov | Production of amorphous water-soluble partially deacetylated chitin |
-
2000
- 2000-04-20 CN CN00114504A patent/CN1112368C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58164601A (en) * | 1982-03-26 | 1983-09-29 | Kohjin Co Ltd | Production of water-soluble chitosan salt |
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| JPH0393902A (en) * | 1989-09-05 | 1991-04-18 | Tokai Riyokaku Tetsudo Kk | Ground coil laying method |
| CN1085564A (en) * | 1993-08-20 | 1994-04-20 | 连云港开发区金祥贸易有限公司 | A kind of preparation method of chitin |
| CN1089620A (en) * | 1993-12-15 | 1994-07-20 | 屈步华 | Preparation method and product with natural structure chitin |
| CN1138336A (en) * | 1994-12-02 | 1996-12-18 | 汉克尔股份两合公司 | Cationic biopolymers |
| JPH115803A (en) * | 1997-06-18 | 1999-01-12 | Tottori Pref Gov | Production of amorphous water-soluble partially deacetylated chitin |
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| Publication number | Publication date |
|---|---|
| CN1318568A (en) | 2001-10-24 |
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