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Crystallization method of cyclic adenosine monophosphate

A technology for cyclic adenosine monophosphate and cyclic adenosine monophosphate sodium salt is applied in the crystallization field of cyclic adenosine monophosphate, which can solve the problems of inconvenient storage, transportation and use, low water content of amorphous products, poor particle size distribution and crystal habit quality, etc. , to achieve the effect of easy industrialized continuous production, good gloss and uniform particle size

Inactive Publication Date: 2013-09-25
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Domestically produced cyclic adenosine monophosphate sodium salt and its cyclic adenosine monophosphate (cAMP-Na / cAMP) are basically amorphous, and the particle size distribution and crystal habit quality of crystalline products are poor, such as poor fluidity, low specific gravity, and amorphous products. The water content is low and unstable, which brings inconvenience to subsequent storage, transportation and use
At present, there is little research on the crystallization process of cyclic adenosine monophosphate sodium salt and its cyclic adenosine monophosphate (cAMP-Na / cAMP), and there is no relevant literature report

Method used

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  • Crystallization method of cyclic adenosine monophosphate
  • Crystallization method of cyclic adenosine monophosphate
  • Crystallization method of cyclic adenosine monophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 500g of anion exchange resin to fill the fixed bed. After equilibrium, put 10L of cAMP fermentation broth with a concentration of about 5.31g / L on the column. After the adsorption is saturated, use high-concentration NaCl and a small amount of hydrochloric acid to elute to obtain high-concentration cyclic adenosine monophosphate. Sodium saline solution.

Embodiment 2

[0031] Take 10ml of cyclic adenosine monophosphate aqueous solution with a concentration of 4g / L, pH=3.01, titrate with 0.01mol / L NaOH solution, the titration result is figure 1 . The marked part is the EP point, which is about pH=8.0.

Embodiment 3

[0033] Add 10L of an aqueous solution with a concentration of 10g / L cyclic adenosine monophosphate sodium salt, pH=8.9, in a water bath controlled at 20°C and a stirring rate of 150rpm, and slowly add 29L of anti-solvent anhydrous ethanol. After the crystallization was complete, the suspension was filtered with suction, washed with a small amount of ethanol to obtain white crystals, and placed in an oven at 45°C for vacuum drying. The single-step crystallization yield was 95.1%, and the purity was 99.1%.

[0034] Take the high-purity cyclic adenosine monophosphate sodium salt that has been crystallized above to prepare 1L of saturated aqueous solution. The water bath is controlled at 20°C and the stirring rate is 120rpm. Slowly add hydrochloric acid to adjust the pH to 4.8. When tiny crystals appear, stop adding Hydrochloric acid, crystal growth at 120rpm stirring speed for 3 hours, continue to drop hydrochloric acid until the pH is 2.0, after the crystallization is complete, ...

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Abstract

The invention discloses a crystallization method of cyclic adenosine monophosphate. The crystallization method comprises the following steps: adding an organic solvent used as an anti-solvent into 10-400g / L of a cyclic adenosine sodium phosphate aqueous solution at pH of 7.0-9.0 under the condition of stirring, carrying out pumping filtration after crystallization is completely finished, washing crystals by the use of ethanol, and carrying out vacuum drying to obtain cyclic adenosine sodium phosphate crystals; dissolving the above cyclic adenosine sodium phosphate crystals in water to obtain a saturated solution of the cyclic adenosine sodium phosphate crystals, adjusting pH of the solution to 4.0-5.5 by the use of acid while stirring, carrying out crystal growing for 0.5-8h, adjusting pH to 1.0-2.5, carrying out pumping filtration after crystallization is completely finished, washing crystals by the use of ethanol, and carrying out vacuum drying to obtain cyclic adenosine monophosphate crystals. By the adoption of the method provided by the invention, quality of the final product is obviously improved, yield of the crystal product is stably raised, and granular size of the crystals can be controlled by changing crystallization stirring speed or temperature. The method provided by the invention is simple to operate, has good repeatability, and is suitable for industrial production of cyclic adenosine sodium phosphate.

Description

technical field [0001] The invention belongs to the field of biological product processing, and in particular relates to a crystallization method of cyclic adenosine monophosphate. Background technique [0002] Cyclic adenosine monophosphate molecular formula is C10H12N5O6P, molecular weight 329.21; alias: cyclic adenosine monophosphate, 3'-5' cyclic adenosine monophosphate (English 3', 5'cyclic adenosine monophosphate); not very stable in acidic solution; 4 Store dry at ℃. The molecular structural formula of cyclic adenosine monophosphate is as follows. [0003] [0004] Cyclic adenosine monophosphate is a white or off-white powder; it is odorless with a slightly salty taste; it is slightly soluble in water and almost insoluble in ethanol or ether. Calculated according to the mass of the dry product, the content of cyclic adenosine monophosphate should be 97.0% to 103.0%. [0005] In 1957, Sutherland discovered cyclic AMP (cAMP). He identified cAMP as a factor that a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/213C07H1/06
Inventor 应汉杰李人杰吴菁岚温庆仕钱文斌庄伟陈勇谢婧婧陈晓春
Owner NANJING UNIV OF TECH
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