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A kind of purification method of enramycin

A technology of enramycin and purification method, applied in the direction of peptides and the like

Active Publication Date: 2018-06-26
CHINA ANIMAL HUSBANDRY IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a new method for obtaining enramycin by silica gel column chromatography purification, so as to overcome a series of problems in the existing enramycin purification process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Fully mix 500g of enramycin flash powder with 1.5L of methanol to obtain a mixture, use 0.1mol / L of hydrochloric acid in methanol solution to adjust the pH of the mixture to 1.0, shake fully, and centrifuge at 3000rpm for 30min to obtain the supernatant to make En Laramycin extract, utilize the methanol solution of 0.1mol / L sodium hydroxide to adjust the pH of the extract to 6.5, the quality of its dry matter is about 50g (weigh the quality of the rotary steamer first, then use the rotary steamer bottle rotary steaming extract, when no more liquid is evaporated, weigh the mass of the rotary steaming bottle at this time, and subtract the two masses to obtain a dry substance mass of 50g.), then redissolve the dry substance with 500ml methanol, and ultrasonically Shake to fully dissolve, mix 150 g of 300-mesh column chromatography silica gel with the enramycin extract obtained after reconstitution, and dry-load the sample after rotary evaporation at 35°C. When loading the ...

Embodiment 2

[0061] Fully mix 1000g of enramycin flash powder with 4L of methanol to obtain a mixture, adjust the pH of the mixture to 2.0 with 0.5mol / L of hydrochloric acid in methanol, shake fully, and centrifuge at 3000rpm for 30min to obtain the supernatant to make Enla Mycin extract, the methanol solution of potassium hydroxide of 0.5mol / L is used to adjust the pH of the extract to 7.5, and the quality of its dry matter is about 120g, (weigh the quality of the rotary steamer first, then utilize the rotary steamer Rotary evaporation extract, when no more liquid is evaporated, weigh the mass of the rotary evaporation bottle at this time, and subtract the two masses to obtain a dry substance mass of 120g.), then redissolve the dry substance with 1500ml methanol, and ultrasonically oscillate After fully dissolving, 500 g of 100-200 mesh column chromatography silica gel and the enramycin extract obtained after reconstitution were fully mixed, and then dried by rotary evaporation at 40°C and...

Embodiment 3

[0067] Fully mix 1500g of enramycin flash powder with 6L of methanol to obtain a mixture, adjust the pH of the mixture to 4.0 with a methanol solution of 1mol / L hydrochloric acid, shake fully, and centrifuge at 3000rpm for 30min to obtain the supernatant to make Enla Mycin extract, the methanol solution of 1mol / L sodium hydroxide is used to adjust the pH of the extract to 8.5, the quality of its dry matter is about 150g, (weigh the quality of the rotary steamer first, then use the rotary steamer to spin Evaporate the extract, and when no more liquid is evaporated, weigh the mass of the rotary steamer at this time, and subtract the two masses to obtain a dry substance mass of 150g.), then redissolve the dry substance with 2000ml methanol, and ultrasonically oscillate fully Dissolve, fully mix 750g of 200-300 mesh column chromatography silica gel with the enramycin extract obtained after reconstitution, and dry-load the sample after rotary evaporation at 50°C. When loading the s...

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Abstract

The invention provides a purifying method of enramycin. The purifying method comprises the steps of regulating the pH value of a flash powder mixture of methanol and enramycin by using hydrochloric acid to be acidic to obtain an enramycin extracting solution; then, regulating the pH value of the enramycin extracting solution to be neutral, and sequentially eluting by taking column-layer chromatographic silica gel as a separating medium and taking petroleum ether, ethyl acetate, butyl acetate and methanol as eluants to remove impurities; next, eluting enramycin by using a methanol solution of hydrochloric acid to obtain an eluant containing enramycin; and carrying out rotary evaporation and drying after regulating the pH value of the eluant containing enramycin to be neutral to obtain enramycin. By using the method provided by the invention, the impurities can be effectively removed, and defects in the existing purifying method of enramycin can be overcome; experiments prove that the content of enramycin can be up to more than 98% if enramycin is prepared by using the method provided by the invention.

Description

technical field [0001] The invention belongs to the field of antibiotic purification, and mainly relates to a method for purifying enramycin. Background technique [0002] Enramycin, also known as enramycin, enramycin, anlemycin, and persistent mycin, is a polypeptide antibiotic composed of 13 different types of 17 amino acid molecules and fatty acid molecules. A cyclic polypeptide structure is formed, and the fatty acid is located at the end of the polypeptide structure. According to the different types of terminal fatty acids, it is divided into enramycin A and enramycin B, and enramycin is mainly composed of these two components. Enramycin has significant antibacterial effect on Gram-positive bacteria, is not easy to produce drug resistance, can change the distribution of bacterial colonies in the intestinal tract, is beneficial to the digestion and absorption of feed nutrients, and has a good growth-promoting effect. Enramycin hydrochloride is white crystalline powder,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/08C07K1/16
Inventor 吴家鑫徐金雷张传良张国栋齐鹏梁景乐张刚
Owner CHINA ANIMAL HUSBANDRY IND
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