CN104530261A - Method for reducing absorbancy of heparin sodium at 260nm - Google Patents
Method for reducing absorbancy of heparin sodium at 260nm Download PDFInfo
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- CN104530261A CN104530261A CN201410813615.6A CN201410813615A CN104530261A CN 104530261 A CN104530261 A CN 104530261A CN 201410813615 A CN201410813615 A CN 201410813615A CN 104530261 A CN104530261 A CN 104530261A
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- heparin sodium
- absorbancy
- sodium
- method reducing
- ethanol
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Abstract
The invention discloses a method for reducing absorbancy of heparin sodium at 260nm. Solution obtained by carrying out enzymolysis on a heparin sodium crude product is further precipitated, oxidized and then precipitated by adopting hot ethanol, proteins such as nucleic acid, protein and the like with extremely low content in a product can be effectively removed, and the absorbancy of the product at 260nm is reduced. The method for reducing the absorbancy of the heparin sodium at 260nm is simple to operate, obvious in effect and applicable to industrial production.
Description
Technical field
The invention belongs to biological technical field, particularly a kind of method reducing heparin sodium 260nm absorbancy.
Background technology
Heparin sodium is at present in the world the most effectively and the maximum anticoagulation medicine of quantity, it is the sodium salt of the CSSO3 extracted in the intestinal mucosa by pig or ox, belong to mucopolysaccharide material, polysaccharose substance often with albumen, nucleic acid substances etc. are present in biomacromolecule with the form of mixture, and these albumen and nucleic acid have maximum absorption at 260nm place, thus have impact on the quality product of heparin sodium.Therefore, in order to reduce the light absorption value of heparin sodium 260nm, must by these Impurity removals.
Summary of the invention
The invention provides a kind of method reducing heparin sodium 260nm absorbancy, compared with the prior art the present invention has following distinguishing feature and positively effect: the present invention uses hot ethanol precipitation to be brought in waste ethanol by the impurity such as protein, nucleic acid, reduce the 260nm absorbancy of heparin sodium intermediate, method is simple, easy to operate, adopt the heparin sodium intermediate stable in properties that the inventive method obtains, 260nm absorbancy≤0.1.
The present invention adopts following technical scheme to be achieved:
Reduce a method for heparin sodium 260nm absorbancy, comprise the steps:
(1) solution after taking heparin sodium crude product enzymolysis, adds sodium-chlor in 18 ~ 25g/L ratio, after stirring and dissolving, by hydrochloric acid soln adjust ph 9.5 ~ 11.5, stir while add 95% alcohol settling, the precipitation number of degrees are 40 ~ 45%(20 DEG C)
(2) upper strata waste ethanol is extracted into ethanol withdrawing can, lower sediment adds purified water and dissolves, and by sodium hydroxide solution adjust ph 10 ~ 12, adds hydrogen peroxide oxidation 8 ~ 10 hours in 2 ~ 4% ratios.
(3), after oxidation terminates, adding sodium-chlor in 15 ~ 20g/L ratio and dissolve, is 5.0 ~ 6.0 by hydrochloric acid soln adjust ph, stir while add 95% hot ethanol precipitation, the alcohol settling number of degrees 45 ~ 50%(20 DEG C), precipitation temperature is 40 ~ 45 DEG C, sedimentation time 10 ~ 12 hours.
(4) upper strata waste ethanol is extracted into ethanol withdrawing can.Lower sediment, sampling detects.
Embodiment
(1) the solution 500L after taking heparin sodium crude product enzymolysis, adds 10 ㎏ sodium-chlor, after stirring and dissolving, by hydrochloric acid soln adjust ph 9.5 ~ 11.5, stirs while add the alcohol settling 10 hours of 95% of 400L.
(2) upper strata waste ethanol is extracted into ethanol withdrawing can, lower sediment adds purified water and dissolves, and by sodium hydroxide solution adjust ph 10 ~ 12, adds hydrogen peroxide 15L and is oxidized 8 hours.
(3) after oxidation terminates, adding sodium-chlor 10 ㎏ and dissolve, is 5.0 ~ 6.0 by hydrochloric acid soln adjust ph, and stir while add the 95% hot ethanol precipitation of 560L, precipitation temperature is 45 DEG C, sedimentation time 10 hours.
(4) upper strata waste ethanol is extracted into ethanol withdrawing can.Lower sediment, sampling detects.
Claims (9)
1. reduce a method for heparin sodium 260nm absorbancy, it is characterized in that comprising the steps:
Solution after taking heparin sodium crude product enzymolysis, it is appropriate to add sodium-chlor, after stirring and dissolving, uses hydrochloric acid soln adjust ph, stir while add 95% alcohol settling;
Upper strata waste ethanol is extracted into ethanol withdrawing can, and lower sediment adds purified water and dissolves, and uses sodium hydroxide solution adjust ph, adds hydrogen peroxide oxidation;
After oxidation terminates, add sodium-chlor in right amount, use hydrochloric acid soln adjust ph, stir while add 95% hot ethanol precipitation;
Upper strata waste ethanol is extracted into ethanol withdrawing can;
Lower sediment, sampling detects.
2. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the sodium-chlor usage quantity described in step (1) is 18 ~ 25g/L.
3. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the solution ph described in step (1) is 9.5 ~ 11.5.
4. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the alcohol settling number of degrees described in step (1) are 40 ~ 45%(20 DEG C), sedimentation time 10 ~ 12 hours.
5. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the pH value described in step (2) is 10 ~ 12.
6. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the oxidizing condition described in step (2) is: hydrogen peroxide consumption is 2 ~ 4% of liquor capacity, oxidization time 8 ~ 10 hours.
7. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the sodium-chlor consumption described in step (3) is 15 ~ 20g/L.
8. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the pH value described in step (3) is 5.0 ~ 6.0.
9. a kind of method reducing heparin sodium 260nm absorbancy according to claim 1, is characterized in that: the deposition condition described in step (3) is: the alcohol settling number of degrees 45 ~ 50%(20 DEG C), precipitation temperature is 40 ~ 45 DEG C, sedimentation time 10 ~ 12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410813615.6A CN104530261A (en) | 2014-12-24 | 2014-12-24 | Method for reducing absorbancy of heparin sodium at 260nm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410813615.6A CN104530261A (en) | 2014-12-24 | 2014-12-24 | Method for reducing absorbancy of heparin sodium at 260nm |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104530261A true CN104530261A (en) | 2015-04-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410813615.6A Pending CN104530261A (en) | 2014-12-24 | 2014-12-24 | Method for reducing absorbancy of heparin sodium at 260nm |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575385A (en) * | 2008-05-09 | 2009-11-11 | 青岛九龙生物医药有限公司 | Method for separating chondroitin polysulfate from heparin sodium by extraction method |
| CN102603926A (en) * | 2012-03-27 | 2012-07-25 | 烟台东诚生化股份有限公司 | New preparing process of high-titer heparin sodium |
| CN102952204A (en) * | 2012-10-09 | 2013-03-06 | 江苏联众肠衣有限公司 | Novel production technique of heparin sodium |
| CN103145878A (en) * | 2012-12-08 | 2013-06-12 | 青岛九龙生物医药有限公司 | Ultralow heparin sodium technical study |
| CN103804520A (en) * | 2013-11-22 | 2014-05-21 | 青岛九龙生物医药有限公司 | Method for improving test index of heparin sodium competitive product 260nm absorbancy |
| CN104140478A (en) * | 2013-05-08 | 2014-11-12 | 清华大学 | Fine heparin and preparation method of fine heparin |
-
2014
- 2014-12-24 CN CN201410813615.6A patent/CN104530261A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575385A (en) * | 2008-05-09 | 2009-11-11 | 青岛九龙生物医药有限公司 | Method for separating chondroitin polysulfate from heparin sodium by extraction method |
| CN102603926A (en) * | 2012-03-27 | 2012-07-25 | 烟台东诚生化股份有限公司 | New preparing process of high-titer heparin sodium |
| CN102952204A (en) * | 2012-10-09 | 2013-03-06 | 江苏联众肠衣有限公司 | Novel production technique of heparin sodium |
| CN103145878A (en) * | 2012-12-08 | 2013-06-12 | 青岛九龙生物医药有限公司 | Ultralow heparin sodium technical study |
| CN104140478A (en) * | 2013-05-08 | 2014-11-12 | 清华大学 | Fine heparin and preparation method of fine heparin |
| CN103804520A (en) * | 2013-11-22 | 2014-05-21 | 青岛九龙生物医药有限公司 | Method for improving test index of heparin sodium competitive product 260nm absorbancy |
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Application publication date: 20150422 |
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| WD01 | Invention patent application deemed withdrawn after publication |