Preparation method of powdery cytidine triphosphate or sodium salt of cytidine triphosphate

A cytidine triphosphate, powdered technology is applied in the field of preparation of powdered cytidine triphosphate or its sodium salt, and can solve the problems of long refining time, manual grinding and the like

Inactive Publication Date: 2015-04-29
SHANGHAI YOUKESAI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Most of the existing refining methods of cytidine disodium tr...

Method used

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  • Preparation method of powdery cytidine triphosphate or sodium salt of cytidine triphosphate
  • Preparation method of powdery cytidine triphosphate or sodium salt of cytidine triphosphate

Examples

Experimental program
Comparison scheme
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Embodiment approach

[0019] The first is to mix and precipitate an acidic solution containing cytidine triphosphate or its sodium salt with 5-20 times the volume of methanol to obtain powdered cytidine triphosphate or its sodium salt;

[0020] A second embodiment includes the steps of:

[0021] In the first step, the acidic solution containing cytidine triphosphate or its sodium salt is mixed with 2-20 times the volume of the first organic solvent to obtain the first precipitate;

[0022] In the second step, the first precipitate and 2-20 times the volume [volume of ethylene glycol or glycerol (ml): cytidine triphosphate or its sodium salt solution converted to pure weight (g) = 2-20 times] Ethylene glycol or glycerol mixed to obtain a solution;

[0023] In the third step, the solution is mixed with 2-20 times the volume of the second organic solvent and precipitated to obtain powdered cytidine triphosphate or its sodium salt.

[0024] The pH of the acidic solution containing cytidine triphospha...

Embodiment 1

[0046] Weigh 20g CTP, add 1mol / L NaCl solution to dissolve and dilute to 100ml, the resulting solution A 271 is 4300, and the pH is about 3.0. The above CTP solution was slowly added dropwise to 500ml of methanol, and a CTP precipitate was formed. After suction filtration, anhydrous ether was added to the filter cake to remove water, and suction filtration was performed again, and the final wet powder was vacuum-dried (pentoxide Diphosphorus is used as a desiccant, and the vacuum degree is -0.1Mpa).

[0047]The parameters of the CTP product obtained by the method of this embodiment: HPLC: 97.1%; refined quality yield: 96%.

Embodiment 2

[0049] Weigh 20g CTP, add 1mol / L NaCl solution to dissolve and dilute to 100ml, the resulting solution A 271 It is 4320, and the pH is about 3.0.

[0050] Primary precipitation: Add 300ml of 95% ethanol to the above CTP solution, leave it for more than 4 hours, and viscous precipitation will occur.

[0051] Secondary precipitation: dissolve the above precipitate with 40ml ethylene glycol, then slowly add the solution dropwise to 120ml absolute ethanol, and a CTP precipitate will form.

[0052] After suction filtration, add 40ml of absolute ethanol to the filter cake for washing, then suction filtration again, add anhydrous ether to the filter cake to remove moisture and suction filtration, and vacuum dry the final wet powder (phosphorus pentoxide is the desiccant, The vacuum is -0.1Mpa).

[0053] The parameters of the CTP product obtained by the method of this example: HPLC: 96.6%, and the refined mass yield: 94%.

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Abstract

The invention discloses a preparation method of powdery cytidine triphosphate or a sodium salt of cytidine triphosphate. The preparation method comprises the following steps: mixing and precipitating an acid solution containing cytidine triphosphate or the sodium salt of cytidine triphosphate with methanol of which the volume is 5-20 times of that of the acid solution so as to obtain powdery cytidine triphosphate or the sodium salt of powdery cytidine triphosphate, or the preparation method comprises the following steps: (1) mixing the acid solution containing cytidine triphosphate or the sodium salt of cytidine triphosphate with a first organic solvent of which the volume is 2-20 times of that of the acid solution so as to obtain a first precipitate; (2) mixing the first precipitate with ethanediol or glycerin of which the volume is 2-20 times of that of the first precipitate so as to obtain a dissolved solution; (3) mixing and precipitating the dissolved solution with a second organic solvent of which the volume is 2-20 times of that of the dissolved solution so as to obtain powdery cytidine triphosphate or the sodium salt of powdery cytidine triphosphate.

Description

technical field [0001] The invention relates to the field of nucleotide preparation, in particular to a preparation method of powdery cytidine triphosphate or its sodium salt. Background technique [0002] Cytidine 5'-triphosphate (CTP), also known as CTP, is a nucleotide substance existing in the human body, an indispensable substance for life activities, and plays an important role in the normal metabolism of the body In recent years, the medicinal CTP used clinically is cytidine 5'-triphosphate disodium (Cytidine5'-triphosphate disodium), its chemical name is cytidine nucleoside-5'-triphosphate disodium salt, and its branch formula is C 9 h 14 Na 2 o 14 P 3 With a molecular weight of 527.14, it is a nucleotide drug for treating cerebrovascular diseases. Cytidine triphosphate disodium is mainly used for cerebrovascular accident and its sequelae; concussion, traumatic coma, dysfunction after brain surgery; neurosis; cerebrovascular sclerosis, senile dementia; periphera...

Claims

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Application Information

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IPC IPC(8): C07H19/10C07H1/06
Inventor 邵斐傅得响
Owner SHANGHAI YOUKESAI BIOTECH
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