A kind of preparation method of mideamycin

A technology of midecamycin and fermented liquid, which is applied in the field of preparation of high-purity midecamycin, can solve the problems of inability to remove macromolecular soluble proteins, affect product quality and yield, and require a lot of manpower and material resources. White color, simple operation effect

Active Publication Date: 2016-12-07
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method has several disadvantages: 1) Traditional plate and frame filtration consumes a lot of manpower and material resources; 2) Adding zinc sulfate to the pretreatment of the fermentation broth makes the filter residue contain a large amount of toxic element zinc and pollutes the environment; 3) Plate and frame filtration Impurities such as macromolecular soluble proteins, sugars, and pigments cannot be removed, and the quality of the filtrate is poor, and it is prone to emulsification during subsequent extraction, which affects product quality and yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Adjust the midecamycin fermentation broth to pH 4.0 with hydrochloric acid, and put it into a ceramic membrane filter with a pore size of 0.1 μm. After the filtration is completed, in order to ensure the yield, use 2 times the volume of The purified aqueous solution was topped with water, and the filtrate was collected completely. Take 150L of filtrate, adjust the filtrate to pH 8.5 with sodium hydroxide solution, add 15L of butyl acetate, stir evenly and raise the temperature to 45°C, after standing for stratification, midecamycin is transferred to the upper organic phase, and the lower layer of filtrate is discarded. Add about 3 L of oxalic acid solution with a pH of 2.0 to 2.5, stir evenly and let it stand for stratification, then transfer the midecamycin to the lower aqueous phase, and separate the lower solution. Adjust the phase inversion liquid with sodium hydroxide solution to a pH of 8.0, add 400ml of butyl acetate, and extract at 45°C. After obtaining the extr...

Embodiment 2

[0027] Adjust the midecamycin fermentation broth to pH 5.0 with hydrochloric acid, and put it into a ceramic membrane filter with a pore size of 0.1 μm. After the filtration is completed, in order to ensure the yield, use 2 times the volume of The purified aqueous solution was topped with water, and the filtrate was collected completely. Take 100L of filtrate, adjust the filtrate to pH 9.0 with sodium hydroxide solution, add 15L of butyl acetate, stir evenly and raise the temperature to 50°C, after standing for stratification, midecamycin is transferred to the upper organic phase, and the lower layer of filtrate is discarded. Add 3 L of hydrochloric acid solution with a pH of 2.0 to 2.5, stir evenly and let it stand for stratification, then transfer the midecamycin to the lower aqueous phase, and separate the lower layer solution. Adjust the phase inversion liquid with sodium hydroxide solution to a pH of 8.5, add 450ml of butyl acetate, and extract at 50°C. After obtaining th...

Embodiment 3

[0029] Adjust the midecamycin fermentation broth to pH 4.5 with sulfuric acid, and put it into a ceramic membrane filter with a pore size of 0.1 μm. After the filtration is completed, in order to ensure the yield, use 2 times the volume of The purified aqueous solution was topped with water, and the filtrate was collected completely. Take 500L of filtrate, adjust the filtrate to pH 8.7 with sodium hydroxide solution, add 75L of butyl acetate, stir evenly and raise the temperature to 48°C, after standing for stratification, midecamycin is transferred to the upper organic phase, and the lower layer of filtrate is discarded. Add 15L of sulfuric acid solution with a pH of 2.0 to 2.5, stir evenly and let it stand for stratification, then transfer the midecamycin to the lower aqueous phase, and separate the lower layer solution. Adjust the phase inversion solution with sodium hydroxide solution to a pH of 8.3, add 2000ml of butyl acetate, and extract at 48°C. After obtaining the ext...

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Abstract

The invention relates to a method for preparing antibiotic, and particularly relates to a method for preparing high-purity midecamycin. The method comprises steps of directly filtering midecamycin fermentation liquid through a ceramic membrane filter; extracting the filtrate and inverting phase; finally crystallizing the phase inversion liquid through a special crystallization method, then separating crystallized suspension by a centrifugal machine, drying the crystal so as to obtain finished product high-purity midecamycin. The method has the advantages and positive effects of having rapid filtering speed, obtaining high-quality filtrate and high-quality finished product, having high yield, being convenient, and being applicable to industrial production.

Description

technical field [0001] The invention belongs to the field of pharmacy and relates to a method for preparing antibiotics, in particular to a method for preparing high-purity midecamycin. Background technique [0002] The molecular formula of Midecamycin is C 41 h 67 NO 15 , with a molecular weight of 813.97, is a 16-membered macrolide antibiotic. [0003] The traditional method to produce midecamycin is to add zinc sulfate and yellow blood salt to the fermented liquid for plate-and-frame press filtration. After extraction and phase inversion, the press-filtered liquid is heated and crystallized under alkaline conditions, and the crystals are separated and dried to obtain the finished product. The traditional method has several disadvantages: 1) Traditional plate and frame filtration consumes a lot of manpower and material resources; 2) Adding zinc sulfate to the pretreatment of the fermentation broth makes the filter residue contain a large amount of toxic element zinc and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 肖祖梅张洪兰
Owner NEW FOUNDER HLDG DEV LLC
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