CN106977625A - A kind of liquaemin discoloration method - Google Patents
A kind of liquaemin discoloration method Download PDFInfo
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- CN106977625A CN106977625A CN201710337631.6A CN201710337631A CN106977625A CN 106977625 A CN106977625 A CN 106977625A CN 201710337631 A CN201710337631 A CN 201710337631A CN 106977625 A CN106977625 A CN 106977625A
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- liquaemin
- sodium
- solution
- stirring
- filtrate
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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
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0063—Glycosaminoglycans or mucopolysaccharides, e.g. keratan sulfate; Derivatives thereof, e.g. fucoidan
- C08B37/0075—Heparin; Heparan sulfate; Derivatives thereof, e.g. heparosan; Purification or extraction methods thereof
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of liquaemin discoloration method, belong to heparin sodium purification method and technology field, it includes liquaemin being dissolved with water；The pH of heparin sodium aqua is adjusted with hydrochloric acid；Add sodium sulfite stirring reaction 0.6h；Mass concentration is added after 1.5% diatomite, to filter and collect filtrate；Filtrate pH is adjusted to 4.5 using sodium hydroxide solution；It is that 0.8%EDTA reacts 2h to add mass concentration；Add 3% solid sodium chloride；It is 75 DEG C to keep solution temperature, 0.9 times of ethanol of addition, and being passed through cooling water after stirring 0.6h makes greenhouse cooling to 30 DEG C；Obtained mixture is staticly settled, upper strata waste ethanol is pumped, to lower sediment thing dehydration, heparin sodium product is dried to obtain.The metal bridge that the present invention can be destroyed effectively between liquaemin and protein impurities and ferro element, and liquaemin structure is not destroyed, the activity to liquaemin destroys small, steady quality, high income.
Description
Technical field
The present invention relates to a kind of liquaemin discoloration method, the color of liquaemin can be effectively removed, belongs to heparin sodium purification side
Law technology field.
Background technology
Liquaemin is clinically to use most, widest anti-coagulants, and the composite form with albumen goes out in vivo
It is existing.Common liquaemin separate mode has enzymolysis or salt solution, alcohol precipitation, oxidation etc., source and extracting mode due to heparin, slightly
Necessarily contain substantial amounts of nucleic acid and protein impurities, deeper color in product heparin.
The raw materials for production of country's liquaemin are mainly chitterlings at present, and the color of liquaemin is produced and protein impurities and blood
Ferro element in liquid has direct relation, these impurity can with liquaemin formation metal bridge, using common removing protein mode or
It is directly added into metal chelating agent removing effects unobvious, it is the step of causing the direct bleaching in subtractive process, such as universal
Potassium permanganate oxidation, hydrogen peroxide oxidation or the mode associated with both of use, the usage amount of oxidant are larger, to liquaemin
Structure forms destruction, reduces the quality and yield of product.
The content of the invention
Liquaemin activity, steady quality are not interfered with it is an object of the invention to provide one kind, the liquaemin of high income takes off
Color method.
A kind of liquaemin discoloration method that the present invention is used, including：Liquaemin is dissolved with water, the liquaemin finally given
Solution concentration is 8000IU/ml；The pH of resulting heparin sodium aqua is adjusted to 2.5 using hydrochloric acid；Resulting solution side is stirred
Side adds sodium sulfite, stirring reaction 0.6h；It is 1.5% diatomite that mass concentration is added into obtained solution, filters and collects
Filtrate；Filtrate obtained by being adjusted using sodium hydroxide solution, is adjusted while stirring, makes pH=4.5；Matter is added in obtained solution
Amount concentration is 0.8%EDTA, reacts 2h；% solid sodium chlorides are added in obtained solution, stirring dissolves solid sodium chloride；Will
The temperature of the solution arrived is kept for 65 DEG C, is passed through cooling water after adding 0.9 times of ethanol, stirring 0.6h, is made resulting solution greenhouse cooling
To 30 DEG C；Obtained mixture is staticly settled, the supernatant liquor after precipitation is waste ethanol, lower sediment thing for containing liquaemin
Mixture, pumps upper strata waste ethanol, to lower sediment thing dehydration, is dried to obtain heparin sodium product；The matter of the sodium sulfite of addition
It is 1.5% to measure concentration；It is collected by filtration after filtrate, the residual potency rinsed with water in diatomite, residual potency is collected and is mixed into
In collected filtrate；While 0.6%EDTA is added, solution is heated to 60 DEG C, solution is kept 70 DEG C of reaction 2h.
The pH of heparin sodium aqua is adjusted to acidity using hydrochloric acid the beneficial effects of the invention are as follows the present invention, portion can either be made
Divide impurity denaturation, play the effect of removing protein, can remove ferro element creation environmental condition to be follow-up again.By pre-treatment
Heparin solution, can be good at removing ferro element under sodium sulfite and metal chelating agent EDTA combination effect, serves list
The effect that one addition complexing agent is unable to reach.The present invention promotes metal chelating agent to play a role, effectively by adjusting reaction environment
The metal bridge destroyed between liquaemin and protein impurities and ferro element, and liquaemin structure is not destroyed, then removing removing protein
Impurity with removing while ferro element, effectively reduction it is follow-up refined during oxidant consumption, reduce the broken of liquaemin activity
Bad, stabilised quality improves yield.
Embodiment
With reference to specific embodiment, the present invention is described in detail.The liquaemin discoloration method of the present embodiment, including
Following steps：Liquaemin is dissolved with water, the heparin sodium aqua concentration finally given is 8000IU/ml；Using hydrochloric acid by gained
To the pH of heparin sodium aqua be adjusted to 2.5；Resulting solution is added into sodium sulfite, stirring reaction 0.6h while stirring；To obtaining
Solution in add mass concentration be 1.5% diatomite, filter and collect filtrate；Filter obtained by being adjusted using sodium hydroxide solution
Liquid, is adjusted while stirring, makes pH=4.5；It is 0.8%EDTA that mass concentration is added in obtained solution, reacts 2h；Obtained solution
Middle addition % solid sodium chlorides, stirring dissolves solid sodium chloride；The temperature of obtained solution is kept for 65 DEG C, 0.9 times of second is added
Cooling water is passed through after alcohol, stirring 0.6h, makes resulting solution greenhouse cooling to 30 DEG C；Obtained mixture is staticly settled, precipitated
Supernatant liquor afterwards be waste ethanol, lower sediment thing be the mixture containing liquaemin, upper strata waste ethanol is pumped, to lower sediment thing
It is dehydrated, is dried to obtain heparin sodium product；The mass concentration of the sodium sulfite of addition is 1.5%；It is collected by filtration after filtrate, is rushed with water
The residual potency washed in diatomite, will remain potency and collects and be mixed into collected filtrate；Adding the same of 0.6%EDTA
When, solution is heated to 60 DEG C, solution is kept 70 DEG C of reaction 2h.
The result that heparin sodium product is obtained to the present embodiment is analyzed：The percentage and quiet reduced to liquaemin color
The reduction ratio of potassium permanganate usage amount is tested during putting.Through detection this embodiment method colour removal rate
For 35%.By using the treated product of the present invention, decolourized using potassium permanganate oxidation, use UV spectrophotometer measuring
OD400nm numerical value, by this index display color index, is as a result shown on the basis of making color up to standard, potassium permanganate
Consumption reduces 60%.
The above described is only a preferred embodiment of the present invention, being not the limitation for making other forms to the present invention, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But it is every without departing from technical solution of the present invention content, the technical spirit according to the present invention is to above example institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.
Claims (1)
1. a kind of liquaemin discoloration method, it is characterised in that it comprises the following steps：Liquaemin is dissolved with water, finally given
Heparin sodium aqua concentration be 8000IU/ml；The pH of resulting heparin sodium aqua is adjusted to 2.5 using hydrochloric acid；Gained is molten
Liquid adds sodium sulfite, stirring reaction 0.6h while stirring；It is 1.5% diatomite, mistake that mass concentration is added into obtained solution
Filter and collect filtrate；Filtrate obtained by being adjusted using sodium hydroxide solution, is adjusted while stirring, makes pH=4.5；Obtained solution
Middle addition mass concentration is 0.8%EDTA, reacts 2h；% solid sodium chlorides are added in obtained solution, stirring makes solid sodium chloride
Dissolving；The temperature of obtained solution is kept for 65 DEG C, cooling water is passed through after adding 0.9 times of ethanol, stirring 0.6h, makes resulting solution
Greenhouse cooling is to 30 DEG C；Obtained mixture is staticly settled, the supernatant liquor after precipitation be waste ethanol, lower sediment thing be containing
The mixture of liquaemin, pumps upper strata waste ethanol, to lower sediment thing dehydration, is dried to obtain heparin sodium product；The sulfurous of addition
The mass concentration of sour sodium is 1.5%；It is collected by filtration after filtrate, the residual potency rinsed with water in diatomite, residual potency is collected
And be mixed into collected filtrate；While 0.6%EDTA is added, solution is heated to 60 DEG C, solution is kept for 70 DEG C instead
Answer 2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710337631.6A CN106977625A (en) | 2017-05-15 | 2017-05-15 | A kind of liquaemin discoloration method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710337631.6A CN106977625A (en) | 2017-05-15 | 2017-05-15 | A kind of liquaemin discoloration method |
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| Publication Number | Publication Date |
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| CN106977625A true CN106977625A (en) | 2017-07-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710337631.6A Withdrawn CN106977625A (en) | 2017-05-15 | 2017-05-15 | A kind of liquaemin discoloration method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909288A (en) * | 2020-08-13 | 2020-11-10 | 山东辰龙药业有限公司 | Refining method of heparin sodium |
-
2017
- 2017-05-15 CN CN201710337631.6A patent/CN106977625A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909288A (en) * | 2020-08-13 | 2020-11-10 | 山东辰龙药业有限公司 | Refining method of heparin sodium |
| CN111909288B (en) * | 2020-08-13 | 2021-09-03 | 山东辰龙药业有限公司 | Refining method of heparin sodium |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170725 |
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| WW01 | Invention patent application withdrawn after publication |