Method for reducing impurities of spiramycin by recrystallization

A technology of spiramycin and recrystallization, which is applied in the field of medicine and chemical industry, can solve the problem that impurities cannot be completely removed, and achieve the effects of low cost, simple process flow and increased purity

Active Publication Date: 2015-04-01
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the abnormal metabolism during the fermentation process, various impurities appear in the fermentation broth, and these impurities cannot be completely removed after solvent extraction and refining

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Potassium dihydrogen phosphate is dissolved in deionized water at a mass dissolution rate of 1.0%, and then the pH value of the potassium dihydrogen phosphate solution is adjusted to 2.0 with oxalic acid. (2) According to the solid-state spiramycin mass dissolution rate is 7 × 10 4 μ / ml Add solid spiramycin to the obtained mixed solution, stir and dissolve at 25°C, and the obtained spiramycin solution is obtained. (3) Adding mass concentration in the spiramycin solution is 12% sodium hydroxide solution, the control sodium hydroxide solution adding process time is 30~50min, until the pH value is adjusted to 9.0, then press the heating rate to be 35 ℃ / h The temperature was raised for 90 minutes, and the temperature was kept at 50° C. and stirred for 50 minutes for crystallization. (4) Centrifuge to obtain wet powder, repeat steps (1), (2), and (3) for one time to obtain wet powder, keep the temperature at 30°C and dry for 12 hours to obtain low-impurity spiramycin. ...

Embodiment 2

[0017] (1) Potassium dihydrogen phosphate is dissolved in purified water at a mass dissolution rate of 1.3%, and then the pH value of the potassium dihydrogen phosphate solution is adjusted to 2.5 with oxalic acid. (2) According to the mass dissolution rate of solid spiramycin, it is 9.5×10 4 μ / ml Add solid spiramycin to the resulting mixed solution, stir and dissolve at 33°C, and the resulting spiramycin solution is obtained. (3) Adding mass concentration in the spiramycin solution is 13% sodium hydroxide solution, the control sodium hydroxide solution adding process time is 30~50min, until the pH value is adjusted to 9.2, then press the heating rate to be 45 ℃ / h The temperature was raised for 75 minutes, and the temperature was kept at 65° C. and stirred for 40 minutes for crystallization. (4) Centrifuge to obtain wet powder, repeat steps (1), (2), and (3) twice for wet powder, obtain wet powder again and keep the temperature at 53° C. and dry for 12 hours to obtain low-im...

Embodiment 3

[0019] (1) Potassium dihydrogen phosphate is dissolved in deionized water with a mass dissolution rate of 1.5%, and then the pH value of the potassium dihydrogen phosphate solution is adjusted to 2.0 with oxalic acid. (2) According to the mass dissolution rate of solid spiramycin, it is 1.2×10 5 μ / ml Add solid spiramycin to the resulting mixed solution, stir and dissolve at 40°C, and the obtained is a spiramycin solution. (3) Add a sodium hydroxide solution with a mass concentration of 15% to the spiramycin solution to control the oxidation of the hydroxide The sodium solution was added for 30-50 minutes until the pH value was adjusted to 9.4, then the temperature was raised at a rate of 55°C / h for 60 minutes, and the temperature was kept at 55°C and stirred for 30 minutes for crystallization. (4) Centrifuge to obtain wet powder, repeat steps (1), (2), and (3) for 3 times to obtain wet powder again, keep the temperature at 75° C. and dry for 12 hours to obtain low-impurity spi...

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PUM

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Abstract

The invention relates to a method for reducing impurities of spiramycin by recrystallization. The method comprises the following steps: (1) dissolving monopotassium phosphate in water and then adjusting the pH value to 2-3 by oxalic acid; (2) putting solid spiramycin into a mixed solution obtained the step (1) and stirring to dissolve at 25-40 DEG C; (3) adding a sodium hydroxide solution with mass concentration of 12-15% into the spiramycin solution obtained in the step (2), raising the temperature for 60-90 minutes and then keeping the temperature to 50-65 DEG C and stirring to crystallize; and (4) centrifugalizing and separating to obtain wet powder, repeating the steps (1), (2) and (3) on the wet powder, and drying the wet powder obtained again to obtain the low-impurity spiramycin. According to the method provided by the invention, by changing the addition of monopotassium phosphate and oxalic acid and then re-dissolving the spiramycin finished product into the solution of monopotassium phosphate and oxalic acid to be re-crystalized so as to further remove related substances, the product quality is further improved.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a method for reducing spiramycin impurities through recrystallization. Background technique [0002] Spiramycin base is a multi-component macrolide antibiotic produced by S. ambofacienss. Its molecular structure is a macrolide part containing sixteen skeletons, which is white or light yellow amorphous Substance, bitter in taste, is an alkaline antibiotic. Soluble in chloroform, alcohols, hexanol, ketone, butyl acetate and other organic solvents, slightly soluble in water. Its sulfate is soluble in water and lower alcohols. Its melting points are: SPMI: 134-137°C; SPMⅡ: 130-133°C; SPMⅢ: 128-131°C. There is an ultraviolet absorption peak at 231-232nm. It has a color-forming gene itself, and it turns purple when it encounters concentrated sulfuric acid or hydrochloric acid, and is positive for maltol reaction, ninhydrin reaction, Sakaguchi reaction, biur...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 朱德育杜占彬宋玉忠祝立新苏瑜袁岗徐俊奇赵严博
Owner TOPFOND PHARMA CO LTD
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