CN1089615A - 1,6-hexose diphosphate method for purification - Google Patents
1,6-hexose diphosphate method for purification Download PDFInfo
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- CN1089615A CN1089615A CN 93110526 CN93110526A CN1089615A CN 1089615 A CN1089615 A CN 1089615A CN 93110526 CN93110526 CN 93110526 CN 93110526 A CN93110526 A CN 93110526A CN 1089615 A CN1089615 A CN 1089615A
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- clear liquid
- fdp
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- purification
- ethanol
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Abstract
The present invention is a kind of method for purification of biochemical drug, particularly 1, and the method for purification of 6-hexose diphosphate (FDP).Naturally cooling left standstill the long period after the present invention mainly adopted the FDP clear liquid heat tracing that will produce, used washing with alcohol again, obtained the FDP clear liquid purer, that content is higher after the ultrafiltration, and FDP content is up to also having created condition for further drying more than 70%.The invention solves poor stability, a difficult problem that complex process is loaded down with trivial details, and greatly reduce production cost, be beneficial to big suitability for industrialized production.
Description
The present invention relates to a kind of method of purification of biochemical drug, particularly 1, the method for purification of 6-hexose diphosphate.
At present, the traditional method of purification FDP is to adopt alkaline earth salt and ion exchange resin method separation and Extraction FDP from the FDP clear liquid, this method yield is lower, generally be lower than 50%, make many FDP be wasted, and this method also is subjected to the influence of many unfavourable condition in the industrial applications process, less stable, complex technical process and loaded down with trivial details.German patent DE 3709718A has narrated the method that a kind of FDP purifies, and equally also exists the problems referred to above.
Purpose of the present invention is exactly the defective that will overcome aforesaid method, not only technology is simple, good stability, but also make inorganic phosphorus, F-6-P, G-6-P in the FDP clear liquid continue to be converted to FDP, total recovery is also improved greatly, thereby reduce cost greatly, be beneficial to suitability for industrialized production, improve the purity of FDP simultaneously again greatly.
Other purposes of the present invention and advantage will be elaborated in the following description.
Embodiment 1:
Get 10 liters of reaction solutions, FDP content is 490g, puts it in the retort, uncovered, this reaction solution is heated to 80 ℃, after 5 minutes, stops heating, left standstill 6 hours, measure FDP content this moment is 560g, pours reaction solution into whizzer, obtains clear liquid after centrifugal, in this clear liquid, add volume about 2 times to 95% ethanol of clear liquid, about 15 liters, obtain the white precipitate of FDP, remove unnecessary clear liquid after, add 5 liters of deionized water dissolving white depositions, add 500ml ammonia magnesium solution then, make PH=8, produce white precipitate, with this white precipitate through whizzer centrifugal or vacuum filter filtration treatment, obtain 5 liters of clear liquids, this clear liquid with 2 times of washing with alcohol of 95% to 10 liters of its clear liquid volumes, is extracted the FDP precipitation, to precipitate ethanol repetitive scrubbing again with 50%, again with deionized water dissolving, add small amount of H type 732 resins then with impurity absorption such as positively charged ion and remove, pass through activated carbon treatment more after filtering, by the ultra-fine filter ultrafiltration, obtain the higher FDP clear liquid of purer content.FDP trisodium liquid salt (butt) active constituent content is 98% in the finished product, and inorganic phosphorus≤0.5%, F-6-P, G-6-P total content ∠ 1%, total recovery is 290g/560g=70%.
Claims (1)
1,1,6--hexose diphosphate process for purification refine is characterized in that:
A, the FDP clear liquid is heated to 80 ℃, is incubated 5 minutes;
B, naturally cooling left standstill more than 5 hours;
C, to pour the FDP clear liquid into whizzer centrifugal;
Add 95% ethanol in d, the clear liquid after centrifugal, 2 times of ethanol volumes are to this clear liquid;
E, treat post precipitation, remove unnecessary clear liquid, throw out is dissolved in water;
F, adding ammonia magnesium solution make PH=8, produce white precipitate;
G, white precipitate be centrifugal or vacuum filter processing through whizzer, gets clear liquid;
H, repetition d step;
I, use 50% ethanol repetitive scrubbing again;
J, usefulness deionized water dissolution precipitation thing;
K, add the Hydrogen resin cation (R.C.) and stir, through centrifugal or filter clear liquid;
L, with gac clear liquid is done decolouring and handle;
Clear liquid after m, the decolouring is admitted to ultrafiltration in the ultra-fine filter.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 93110526 CN1089615A (en) | 1993-01-11 | 1993-01-11 | 1,6-hexose diphosphate method for purification |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 93110526 CN1089615A (en) | 1993-01-11 | 1993-01-11 | 1,6-hexose diphosphate method for purification |
Publications (1)
Publication Number | Publication Date |
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CN1089615A true CN1089615A (en) | 1994-07-20 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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CN 93110526 Pending CN1089615A (en) | 1993-01-11 | 1993-01-11 | 1,6-hexose diphosphate method for purification |
Country Status (1)
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CN (1) | CN1089615A (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0814087A2 (en) | 1996-05-08 | 1997-12-29 | Cypros Pharmaceutical Corporation | Partially lyophilized fructose-1,6-diphosphate (FDP) for injection into humans |
US5731291A (en) * | 1996-05-08 | 1998-03-24 | Cypros Pharmaceutical Corp. | Partially lyophilized fructose-1,6-diphosphate (FDP) for injection into humans |
CN1042953C (en) * | 1995-07-10 | 1999-04-14 | 暨南大学 | Magnesium hexose diphosphate and its production |
US6074658A (en) * | 1997-10-03 | 2000-06-13 | Cypros Pharmaceutical Corp. | Treatment of sickle cell anemia crises with fructose-1, 6-diphosphate as an analgesic drug |
US6076528A (en) * | 1996-05-09 | 2000-06-20 | Cypros Pharmaceutical Corp. | Injection of fructose-1,6-diphosphate (FDP) prior to coronary artery bypass grafting surgery |
CN100395252C (en) * | 2006-06-12 | 2008-06-18 | 南京工业大学 | Method for continuous separation of fructose-1,6-diphosphate |
CN1895259B (en) * | 2006-06-26 | 2010-06-30 | 天津南开允公医药科技有限公司 | Preparation of injection for treating cardiovascular disease |
-
1993
- 1993-01-11 CN CN 93110526 patent/CN1089615A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1042953C (en) * | 1995-07-10 | 1999-04-14 | 暨南大学 | Magnesium hexose diphosphate and its production |
EP0814087A2 (en) | 1996-05-08 | 1997-12-29 | Cypros Pharmaceutical Corporation | Partially lyophilized fructose-1,6-diphosphate (FDP) for injection into humans |
US5731291A (en) * | 1996-05-08 | 1998-03-24 | Cypros Pharmaceutical Corp. | Partially lyophilized fructose-1,6-diphosphate (FDP) for injection into humans |
US6076528A (en) * | 1996-05-09 | 2000-06-20 | Cypros Pharmaceutical Corp. | Injection of fructose-1,6-diphosphate (FDP) prior to coronary artery bypass grafting surgery |
US6074658A (en) * | 1997-10-03 | 2000-06-13 | Cypros Pharmaceutical Corp. | Treatment of sickle cell anemia crises with fructose-1, 6-diphosphate as an analgesic drug |
US6312707B1 (en) | 1997-10-03 | 2001-11-06 | Questcor Pharmaceuticals, Inc. | Treatment of sickle cell anemia crises with fructose-1,6-diphosphate as an analgesic drug |
CN100395252C (en) * | 2006-06-12 | 2008-06-18 | 南京工业大学 | Method for continuous separation of fructose-1,6-diphosphate |
CN1895259B (en) * | 2006-06-26 | 2010-06-30 | 天津南开允公医药科技有限公司 | Preparation of injection for treating cardiovascular disease |
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