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Process for extracting colistin sulfate through precipitation method

A technology of colistin sulfate and precipitation method, applied in the field of chemical industry, can solve problems such as unfavorable industrialization promotion, rough operation mode, dark product color, etc., and achieve the effects of easy quality control, overcoming complicated steps, and stable quality.

Active Publication Date: 2013-09-11
HEBEI SHENGXUE DACHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method utilizes the solubility difference between polymyxin and impurities in an acidic environment to achieve the purpose of removing impurities. This method is relatively rough in operation, and the obtained product has dark color and low content, which is not conducive to industrialization.
At present, there is a lack of a method for the separation and purification of colistin sulfate that is easy to operate, stable in effect and low in cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (a) Take 1.8L of colistin fermentation liquid containing polymyxin E, adjust the pH value to 2.5-3.5 with oxalic acid, and filter through a microporous filter to obtain 1.5L of filtrate Ⅰ with a potency of 372,000 u / mL. Wherein, the filter membrane of the microporous filtration device is composed of ceramic membrane elements with 19 holes and a cut-off pore diameter of 100 nm.

[0026] (b) Take 7.5 g of Na respectively 2 EDTA and polyaluminum sulfate were sequentially added to the filtrate I, stirred until dissolved, and reacted at room temperature for 0.5h to obtain a reaction solution.

[0027] (c) Rapidly heat the reaction solution to 85°C and keep it warm for 1 hour; quickly lower the temperature of the reaction solution to 20°C within 0.5~1.0 hour with cooling liquid. Take 1.0 g of perlite as a filter aid, and filter with suction to obtain filtrate II.

[0028] (d) Use 5.0M NaOH solution to adjust the pH value of the above filtrate II to 12.5, react at 60r / min ...

Embodiment 2

[0031] (a) Take 1.3L of colistin fermentation liquid containing polymyxin E, adjust the pH value to 3.7~4.0 with concentrated sulfuric acid, and filter through a microporous filter device to obtain 1L of filtrate I with a potency of 379,000 u / mL. Wherein, the filter membrane of the microporous filtration device is composed of ceramic membrane elements with 9 holes and a cut-off pore diameter of 200 nm.

[0032] (b) Take 10.0 g of Na respectively 2 EDTA and 10.0 g of aluminum sulfate were sequentially added to the filtrate I, stirred until dissolved, and reacted at room temperature for 1 h to obtain a reaction liquid.

[0033] (c) Rapidly heat the reaction solution to 70°C and keep it warm for 0.8h; quickly lower the temperature of the reaction solution to 20°C within 0.5~1.0h with cooling liquid. Take 1.0 g of perlite as a filter aid, and filter with suction to obtain filtrate II.

[0034] (d) Use 5.0M NaOH solution to adjust the pH value of the above filtrate II to 12.5, ...

Embodiment 3

[0037] (a) Take 1.8L of colistin fermentation liquid containing polymyxin E, adjust the pH value to 3.3~3.6 with concentrated sulfuric acid, and filter through a microporous filter device to obtain 1.5L of filtrate Ⅰ with a potency of 360,000 u / mL. Wherein, the filter membrane of the microporous filtration device is composed of ceramic membrane elements with 19 holes and a cut-off pore diameter of 50 nm.

[0038] (b) Take 15.0 g of Na 2 SiO 3 , to prepare a saturated solution, slowly add it to the above filtrate, react at room temperature for 3.5h, and then add 6.0g Na 2 EDTA was reacted at room temperature for 0.5 h to obtain a reaction solution.

[0039] (c) Rapidly heat the reaction solution to 90°C and keep it warm for 1 hour; quickly lower the temperature of the reaction solution to 20°C within 0.5~1.0 hour with cooling liquid. Take 1.0 g of perlite as a filter aid, and filter with suction to obtain filtrate II.

[0040] (d) Adjust the pH value of the above filtrate I...

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Abstract

The invention discloses a process for extracting colistin sulfate through a precipitation method. The process comprises the following steps of: (a) adjusting pH of fermentation liquor containing polymyxin E with oxalic acid or concentrated sulfuric acid, and filtering with a filtering device; (b) adding 0 metal complexing agent and inorganic flocculant to the filtrate, and reacting at normal temperature for 0.5 to 4.0h; (c) heating, cooling, and vacuum-filtering the reactive liquid; (d) adjusting pH of the filtrate above with aqueous alkali, separating the solid from the liquid to obtain a filter cake, dissolving the filter cake with sulfuric acid solution so as to obtain acidizing fluid, adding potassium permanganate and activated carbon to the acidizing fluid respectively, agitating for 0.5 to 2.0 hours, and then vacuum-filtering to obtain colistin sulfate liquid; and (e) centrifugally spray-drying the colistin sulfate liquid. With the adoption of the process, the common problems of the existing process for purifying fermentation liquor that the steps are complicated, the period is long, the labor intensity is relatively high, and the wastewater is difficult to treat and the like can be overcame.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a process method for extracting and separating colistin sulfate from colistin fermentation broth. Background technique [0002] Colistin Sulphate (Colistin Sulphate), also known as colistin sulfate, polymyxin E, etc. It is an alkaline cyclic polypeptide antibiotic obtained from the culture solution of Bacillus polymyxa. It is a mixture of polymyxin E1 and E2. It is a white or off-white powder, easily soluble in water, heat-resistant, and difficult to absorb in the digestive tract. , rapid excretion, less toxic and side effects, less likely to produce drug-resistant strains, is one of the safest growth-promoting antibiotics for livestock and poultry. Colistin sulfate has a strong antibacterial effect on Gram-negative bacteria, and is effective against almost all Gram-negative bacteria, especially sensitive to Pseudomonas aeruginosa, Escherichia coli, Klebsiella pneumoni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/62C07K1/36C07K1/34C07K1/30
Inventor 孟繁珠谷新华常国栋宋志倩
Owner HEBEI SHENGXUE DACHENG PHARMA
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