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A kind of purification method of creatine phosphate sodium and preparation of sterile powder thereof

A technology of sodium creatine phosphate and a purification method, which is applied in the field of preparation of sterile powder

Active Publication Date: 2018-03-13
CHONGQING SHENGHUAXI PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of purity in the purification method, the present invention provides a method of sodium creatine phosphate with convenient operation and good purification effect

Method used

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  • A kind of purification method of creatine phosphate sodium and preparation of sterile powder thereof
  • A kind of purification method of creatine phosphate sodium and preparation of sterile powder thereof
  • A kind of purification method of creatine phosphate sodium and preparation of sterile powder thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 5g of creatine phosphate sodium to the reaction flask, add 50mL of 10M NaOH solution, heat to 80℃, stir for 10h, and detect the HPLC content of sodium creatine phosphate in liquid phase <5.0%, stop heating, cool to 0~5℃, stir for 2h, filter with suction, add 15mL ethanol to the filter cake, stir and wash, filter with suction, and calculate the weight of creatinine sodium phosphate through external standard for the wet solid. Add 14.5 mL of 0.1M sodium hydroxide solution to the wet filter cake and stir at 30°C until the reaction is complete, add 50 mL of acetonitrile, cool to 0~5°C, stir and crystallize for 2h, filter with suction, add acetonitrile to the filter cake, stir and wash until the pH of the washing liquid is 7~8, suction filtered, dried under reduced pressure at 40°C to obtain 4.38g of creatine phosphate refined product, yield 87.6%, HPLC purity 99.81%, creatinine 0.06%, creatine 0.07%, phosphate <0.2%.

Embodiment 2

[0025] Add 5g of creatine phosphate sodium to the reaction flask, add 50mL of 10M NaOH solution, heat to 80℃, stir for 10h, and detect the HPLC content of sodium creatine phosphate in liquid phase <5.0%, stop heating, cool to 0~5℃, stir for 2h, filter with suction, add 15mL ethanol to the filter cake, stir and wash, filter with suction, and calculate the weight of creatinine sodium phosphate through external standard for the wet solid. Add 11.6 mL of 0.5M sodium hydroxide solution to the wet filter cake and stir at 25°C until the reaction is complete, add 100 mL of acetone, cool to 0~5°C, stir and crystallize for 2 hours, filter with suction, add acetone to the filter cake, stir and wash until the pH of the washing liquid is 7~8, filtered by suction, dried under reduced pressure at 40°C to obtain 3.96g of refined creatine phosphate sodium, yield 79.2%, HPLC purity 99.84%, creatinine 0.06%, creatine 0.08%, phosphate <0.2%.

Embodiment 3

[0027] Add 5g of creatine phosphate sodium to the reaction flask, add 50mL of 13M NaOH solution, heat to 70℃, stir for 8h, and detect the HPLC content of sodium creatine phosphate in liquid phase <5.0%, stop heating, cool to 0~5℃, stir for 2h, filter with suction, add 15mL ethanol to the filter cake, stir and wash, filter with suction, and calculate the weight of creatinine sodium phosphate through external standard for the wet solid. Add 7.3 mL of 1.0M sodium hydroxide solution to the wet filter cake and stir at 20°C until the reaction is complete, add 50 mL of methanol, cool to 0~5°C, stir and crystallize for 2h, filter with suction, add methanol to the filter cake, stir and wash until the pH of the washing liquid is 7~8, filtered by suction, dried under reduced pressure at 40°C to get 3.12, yield 62.4%, HPLC purity 99.87%, creatinine 0.04%, creatine 0.04%, phosphate <0.2%.

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Abstract

The invention discloses a phosphocreatine disodium purification method. The method comprises dissolving phosphocreatine disodium in a concentrated sodium hydroxide aqueous solution, heating the solution to transform phosphocreatine disodium into a creatinine phosphate sodium salt, carrying out hydrolysis ring opening on the creatinine phosphate sodium salt, and carrying out crystallization to obtain a phosphocreatine disodium refined product. The method can effectively remove inorganic impurities and inorganic impurities in phosphocreatine disodium and improve product purity. The phosphocreatine disodium refined by the method under aseptic conditions can be directly used for split charging preparation of phosphocreatine disodium aseptic powder.

Description

Technical field [0001] The invention relates to a purification method of raw material medicine creatine phosphate sodium and the preparation of sterile powder thereof. Background technique [0002] Creatine phosphate is an important energy supply substance in myocardial metabolism. It was isolated from mammalian muscle in 1928. Phosphocreatine disodium (phosphocreatine disodium), the chemical name is N-[imino(phosphoamino)methyl]-N-methylglycine disodium salt, the structural formula is shown below is its medicinal form, which has a cardioprotective function, With no side effects, it can be used as an adjuvant therapy for cardiology and surgery. Clinically, it can be used to treat insufficient striated muscle activity as an adjuvant therapy for myocardial diseases. In 1992, the Italian Ouhui Pharmaceutical Factory first developed a new drug for the development of creatine phosphate disodium salt on the market. Because of its definite curative effect and low side effects, it was ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/22
Inventor 王庆
Owner CHONGQING SHENGHUAXI PHARMA CO LTD