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Process for purifying nosiheptide by passing through column

A Nosiheptide and column-passing technology, which is applied in the fields of peptide, organic chemistry, and peptide preparation methods, can solve problems such as difficult to achieve content, difficult to remove Nosiheptide impurities, and Nosiheptide decomposition, so as to achieve less decomposition and avoid Long purification time and obvious effect

Active Publication Date: 2014-12-24
甘肃汇能生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is: it is difficult to remove impurities in nosiheptide in the purification method of nosiheptide in the prior art, it is easy to decompose nosiheptide in the operation process, and the content of nosiheptide product is difficult to reach more than 90%. The problem is to provide a method for purifying nosiheptide through a column, and to achieve the purpose of purification by selecting two kinds of macroporous adsorption resins with different polarities to adsorb impurities in nosiheptide

Method used

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  • Process for purifying nosiheptide by passing through column

Examples

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Comparison scheme
Effect test

Embodiment 1

[0025] The process of column purification of nosiheptide, its concrete steps are as follows:

[0026] (1) Add 2 g of nosiheptide crude product (content 70%) into 30 ml of mixed solvent (acetone:methanol 80% volume ratio 1:1), add acid to adjust the pH value to completely dissolve nosiheptide;

[0027] (2) After the macroporous adsorption resins HPD-100 and HPD-500 were pretreated with acetone and methanol in sequence, they were mixed according to the ratio of 1:2 and then wet-loaded into a chromatography column with a column diameter ratio of 15:1;

[0028] (3) Pass the previously configured nosiheptide solution through the mixed resin column, control the flow rate to 5ml / min, and collect the column liquid;

[0029] (4) Neutralize to neutral with alkali, concentrate under reduced pressure to one-tenth of the original volume, a large amount of solids precipitate out, filter, wash the filter cake with water, and dry under reduced pressure to obtain 1.11g of purified Nosiheptide ...

Embodiment 2

[0031] The process of column purification of nosiheptide, its concrete steps are as follows:

[0032] (1) Add 2 g of nosiheptide crude product (content 70%) into 40 ml of mixed solvent (acetone:methanol 80% volume ratio 1:1), add acid to adjust the pH value to completely dissolve nosiheptide;

[0033] (2) After the macroporous adsorption resins HPD-100 and HPD-500 were pretreated with acetone and methanol respectively, they were mixed according to the ratio of 3:5 and then wet-loaded into a chromatography column with a column diameter ratio of 15:1;

[0034] (3) Pass the previously configured nosiheptide solution through the mixed resin column, control the flow rate to 4ml / min, and collect the column liquid;

[0035] (4) Neutralize to neutral with alkali, concentrate under reduced pressure to one-tenth of the original volume, a large amount of solids precipitate out, filter, wash the filter cake with water, and dry under reduced pressure to obtain 1.14g of purified Nosiheptide...

Embodiment 3

[0037] (1) Add 2 g of nosiheptide crude product (content 70%) into 40 ml of mixed solvent (acetone:methanol 80% volume ratio 1:2), add acid to adjust the pH value to completely dissolve nosiheptide;

[0038] (2) After the macroporous adsorption resins HPD-100 and HPD-500 were pretreated with acetone and methanol in sequence, they were mixed according to the ratio of 3:4 and then wet-loaded into a chromatography column with a column diameter ratio of 15:1;

[0039] (2) Pass the previously configured nosiheptide solution through the mixed resin column, control the flow rate to 2ml / min, and collect the column liquid;

[0040] (3) Neutralize to neutral with alkali, concentrate under reduced pressure to one-tenth of the original volume, a large amount of solids precipitate out, filter, wash the filter cake with water, dry under reduced pressure to obtain 1.15g of purified nosiheptide, content 95.1% , The total recovery rate was 78.11%.

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Abstract

The invention discloses a method for purifying nosiheptide, and particularly relates to a process for purifying nosiheptide by passing through a column. The process comprises the following main steps: preparing a nosiheptide column-passing liquid; and adsorbing, concentrating and drying a macroporous resin column, and the like. According to the method, the purity of a nosiheptide crude product can be effectively improved by selecting proper macroporous resin, a column-passing method and a concentrating and drying method, the content of the prepared nosiheptide can be over 95 percent, and the yield of the nosiheptide can be 70-80 percent. The method has low requirement for instruments and equipment, is simple to operate, and is suitable for large-scale production operation.

Description

technical field [0001] The invention belongs to the technical field of separation engineering and relates to a process for purifying nosiheptide, in particular to a process for purifying nosiheptide by a column passing method. Background technique [0002] Nosiheptide is an animal-specific antibiotic, and its antibacterial mechanism is to inhibit bacterial protein synthesis to play an antibacterial effect. Bacteria are not easy to develop resistance to nosiheptide, and there is no obvious cross-resistance with other antibiotics. Nosiheptide has higher activity against Gram-positive bacteria, especially Staphylococcus. Nosiheptide has low toxicity, and it is seldom absorbed in the digestive tract of animals when administered in mixed feeding, so there are few residues in animal products. [0003] Uses: Antibiotic drugs, used to promote the growth of livestock and poultry. [0004] [0005] Molecular formula: C 51 h 43 N 13 o 12 S 6 [0006] Molecular weight: 1222....

Claims

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Application Information

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IPC IPC(8): C07K5/078C07K1/16
Inventor 徐天华黄振吴中华陈军王丽陈贵才
Owner 甘肃汇能生物工程有限公司
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