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Method for preparing Enramycin A and B hydrochloride mixture

A technology of enramycin and hydrochloride, applied in the field of preparing enramycin A and B hydrochloride mixture, can solve the problems of large-scale production limitation, cumbersome weak acid resin regeneration, high solvent usage, and achieves The effect of long resin life, low cost and low price

Inactive Publication Date: 2013-12-04
SHANGHAI INST OF PHARMA IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese authorized patent CN 101597578B uses macroporous adsorption resins such as Amberlight XAD-4 and XAD-16 and combines solvent, hydrochloric acid and sodium chloride gradient elution to separate and extract enramycin; but its solvent usage is high and the steps are cumbersome , the obtained purity is unknown, and the price of the resin is high, which has a limiting effect on large-scale production
Another Chinese invention patent application 201010213986.2 uses a macroporous weakly acidic cationic resin to separate and extract enramycin; however, the regeneration of the weakly acidic resin is cumbersome, and it also uses a large amount of solvent

Method used

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  • Method for preparing Enramycin A and B hydrochloride mixture
  • Method for preparing Enramycin A and B hydrochloride mixture
  • Method for preparing Enramycin A and B hydrochloride mixture

Examples

Experimental program
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Effect test

Embodiment 1

[0054] 1L enramycin fermented liquid is filtered, obtain the mycelium that contains enramycin, weigh 42g, be 2.0 (with hydrochloric acid to adjust pH) aqueous solution (extract solution) that mycelium contains 50% methanol ) in 200ml, then perform ultrasonic cell disruption for 1h and mechanically stir for 12h, filter after standing, add 100ml of the above extract to the mycelium filter residue, filter after ultrasonic stirring, mix the two filtrates and vacuum at 35°C Concentrate to 30ml to obtain a concentrated solution containing enramycin A and B.

[0055] Install a chromatographic column with a height of 16cm and a diameter of 4cm containing macroporous adsorption resin HZ-816, and regenerate the equilibrium completely. Adjust the pH of the above concentrated solution to 8.0, add 30ml of 50% methanol and filter, put the filtrate on the column at a speed of 50ml / h, and then wash 2CV and 3CV with 20% and 80% aqueous methanol to remove impurities; 60% methanol with pH 2.0 (...

Embodiment 2

[0057] 1L enramycin fermented liquid is filtered, obtain the mycelium that contains enramycin, weighing 52g, the aqueous solution (extract solution) that contains 84% ​​methanol pH is 4.0 (with hydrochloric acid to adjust pH) with mycelium ) in 300ml, then ultrasonically disrupted cells for 1.5h and mechanically stirred for 24h, filtered after standing, and concentrated under reduced pressure and vacuum at 40°C to 20ml to obtain a concentrated solution containing enramycin A and B.

[0058] Install a chromatographic column with a height of 20cm and a diameter of 4cm containing macroporous adsorption resin HZ-818, and regenerate the equilibrium completely. Adjust the pH of the above-mentioned concentrated solution to 9.0, add 20ml of 84% methanol and filter, put the filtrate on the column at a speed of 50ml / h, and then wash 2CV and 3CV with 40% and 70% methanol aqueous solution to remove impurities; The aqueous solution of 90% methanol with a pH of 3.0 (adjusted with hydrochlor...

Embodiment 3

[0060] 1L enramycin fermented liquid is filtered, obtain the mycelium that contains enramycin, weigh 48g, be 3.0 (with hydrochloric acid to adjust pH) aqueous solution (extract solution) that mycelium contains 75% methanol ) in 300ml, then subjected to ultrasonic cell disruption for 2h and mechanical stirring for 18h, filtered after standing, and concentrated under reduced pressure and vacuum at 40°C to 10ml to obtain a concentrated solution containing enramycin A and B.

[0061] Install a chromatographic column with a height of 25cm and a diameter of 4cm containing macroporous adsorption resin HZ-803, and regenerate the equilibrium completely. Adjust the pH of the above concentrate to 8.5, add 10ml of 75% methanol and filter it, put the filtrate on the column at a speed of 50ml / h, then wash 2CV and 3CV with 40% and 70% aqueous methanol to remove impurities; 80% methanol with a pH of 2.5 (adjust the pH with hydrochloric acid) was eluted, and the eluate was collected step by st...

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Abstract

The invention provides a method for preparing an Enramycin A and B hydrochloride mixture. The method comprises the steps that: (1) a fermentation broth comprising Enramycin A and B is separated, such that mycelium is obtained; (2) an extraction liquid with pH regulated to 2.0-4.5 is mixed with the mycelium, wherein the pH is regulated by using hydrochloric acid; ultrasonic crushing is carried out for 1-3h; the mixture is stirred for 12-24h, such that a suspension liquid is obtained; (3) the suspension liquid obtained in the step (2) is sufficiently settled, and filtering is carried out, such that a crude extraction liquid comprising Enramycin A and B hydrochloride is obtained; (4) the crude extraction liquid obtained in the step (3) is subjected to reduced-pressure vacuum concentration under a temperature of 30-40 DEG C, until the volume of the liquid is 1 / 10-1 / 20 of an original volume, such that a concentrate liquid is obtained; (5) the pH of the concentrate liquid obtained in the step (4) is regulated to 8.0-9.0, and the Enramycin A and B hydrochloride is sufficiently dissolved; filtering is carried out, such that mother liquid for column processing is obtained; (6) the mother liquid obtained in the step (5) is processed by using macroporous absorption resin column, such that collected liquid comprising Enramycin A and B hydrochloride mixture is obtained; and (7) the collected liquid obtained in the step (6) is subjected to reduced-pressure vacuum concentration, such that the volume of the liquid is 1 / 50-1 / 100 of an original volume; and lyophilization is carried out, such that the Enramycin A and B hydrochloride mixture is obtained.

Description

technical field [0001] The invention belongs to the field of pharmaceutical engineering, in particular to a method for preparing enramycin A and B hydrochloride mixture. Background technique [0002] Enramycin (English name Enramycin or Enduracidin), also known as Enramycin, Anlemycin, and Duramycin, is a broad-spectrum, efficient and safe new feed additive. It has special effects on Gram-positive bacteria, especially Clostridium perfringens, and has excellent growth-promoting and feed-utilizing effects. It is recommended by many countries in the world as an antibiotic growth-promoting agent for animals. It is a polypeptide antibiotic produced by the fermentation of Actinomyces Streptomyces fungicidious NO.B5477. Enramycin is an organic base composed of 17 amino acid molecules and fatty acid molecules of 13 different types. According to the different types of terminal fatty acids, it can be divided into Enramycin A (Enramycin A, molecular formula: C 107 h 138 Cl 2 N 26...

Claims

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Application Information

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IPC IPC(8): C07K7/08C07K1/16
Inventor 李继安陈代杰陈舟舟尚秀婷钟京谕蓝鸿阚士东
Owner SHANGHAI INST OF PHARMA IND
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