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Crystallization process of 5'-nucleoside sodium triphosphate

A technology of sodium nucleoside triphosphate and nucleoside triphosphate, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as poor product quality, difficult crystallization, and low yield, and achieve product Quality improvement, short crystallization operation time and good reproducibility

Inactive Publication Date: 2006-11-15
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for the production of high-purity 5'-nucleoside triphosphate in aqueous solution to produce high-purity 5'-nucleoside triphosphate in view of the shortcomings of difficult crystallization, poor product quality and low yield in the current 5'-nucleoside triphosphate conventional dissolution method. Crystallization method of nucleoside sodium triphosphate crystal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Two parts of 5'-uridine triphosphate aqueous solution with a concentration of 100g / L, each 10L, were crystallized by conventional elution crystallization and the preparation method of this patent respectively. The former is directly adjusted to pH 8.5 with sodium hydroxide, and 10 L of ethanol is slowly added; the latter is adjusted to pH 7.0 with sodium hydroxide, and 30 g of sodium acetate and 10 L of ethanol are added. The two crystallization process conditions are the same, both are controlled at 25° C., and the stirring speed is 70 rpm. After crystallization, the suspension was filtered with suction, washed with 85% ethanol, and dried in vacuum. Table 1 is a comparison of the product quality and crystallization yield of the two crystallization systems.

[0026] Table 1 Comparison of product quality and crystallization yield of two crystallization systems

[0027] project

Embodiment 2

[0029] Adjust 50L of 5'-uridine triphosphate aqueous solution with a concentration of 300g / L to pH 7.0 with sodium hydroxide, add 400g of sodium acetate and 75L of ether, and control the stirring speed at 20°C to 100rpm. After the crystallization, the suspension was suction-filtered, the resulting white crystals were washed with 85% ethanol, and vacuum-dried to obtain 16.5 kg of 5'-uridine sodium triphosphate crystals. The tested purity of the finished product is 96.3%, the water content is 9.8%, and the final crystallization yield is 91.2%. The test results are shown in Table 2.

[0030] Table 2 The results of quality inspection and analysis of finished products: C 9 h 12 N 2 o 15 P 3 Na 3 (Molecular weight is 550.1)

[0031] Test items

Embodiment 3

[0033] Adjust 10L of 5'-guanosine triphosphate aqueous solution with a concentration of 300g / L to pH 7.5 with sodium hydroxide, add 80g of sodium sulfate, control the stirring speed at 100rpm at 30°C, and add methanol at a flow rate of 1L / h 15L. . After the crystallization, the suspension was suction-filtered, the resulting white crystals were washed with 85% ethanol, and vacuum-dried to obtain 3.53 kg of 5'-guanosine triphosphate sodium salt crystals. The tested purity of the finished product is 97.7%, the water content is 6.6%, and the final crystallization yield is 93.1%. The test results are shown in Table 3.

[0034] Table 3 Results of quality inspection and analysis of finished products: C 10 h 13 N 5 Na 3 o 14 P 3 Na 3 (molecular weight 589.1)

[0035] Test items

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Abstract

A crystallizing process for 5'-nucleoside-sodium triphosphate includes such steps as proportionally adding the inorganic Na salt and solution educing agent, stirring while crystallizing at 15-40 deg.C, filtering, alcohol washing and vacuum drying. It has high output and controllable size of crystal.

Description

technical field [0001] The invention belongs to the technical field of separation and purification engineering, and relates to a crystallization method for producing high-purity 5'-nucleoside sodium triphosphate crystals by using an aqueous solution of 5'-nucleoside triphosphate. Background technique [0002] 5'-nucleoside triphosphate (ATP, CTP, GTP, UTP, hereinafter referred to as UTP) is an important phosphoryl compound, a direct precursor of nucleic acid synthesis, an important coenzyme and energy carrier, and plays a role in the life metabolism of cells. It plays a very important role. Its sodium salt can be used clinically for the treatment and adjuvant therapy of diseases such as heart, brain, blood vessels and nerves, and is also an important raw material for the synthesis of nucleotide derivatives. [0003] Currently commercially available 5'-nucleoside triphosphates are mainly in the form of freeze-dried powder (European Patent EP 1 362 862 A1), with a purity lower...

Claims

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Application Information

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IPC IPC(8): C07H19/10C07H1/06C07H19/20
Inventor 应汉杰吕浩赵谷林
Owner NANJING UNIV OF TECH
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