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Preparation method for preparing vancomycin from 2-methylpyridine

A vancomycin and picoline technology, applied in the direction of peptides, etc., can solve the problems of difficult crystallization, slow growth of vancomycin hydrochloride crystals, difficult crystallization, etc., and achieves simple production method, improved appearance and color, and effective composition. increased effect

Inactive Publication Date: 2017-03-22
江苏海阔生物医药有限公司
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Problems solved by technology

Among them, the crystallization process can improve the purity of vancomycin and remove some impurities such as pigments. However, due to the slow growth of vancomycin hydrochloride crystals, the crystallization process is easily disturbed by impurities, and the crystallization is difficult. Only the crude extract through ion exchange and decolorization hard to crystallize

Method used

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  • Preparation method for preparing vancomycin from 2-methylpyridine

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preparation example Construction

[0020] see figure 1 , the invention provides a kind of preparation method that prepares vancomycin by 2-picoline, comprises the following steps:

[0021] a. Rapidly mixing the antibiotic fermentation mixture with 2-picoline to obtain a solution with a pH value of at least about 7.8, and allowing it to continue to precipitate without stirring;

[0022] b, crystallizing the precipitate formed in step a from the solution;

[0023] c. The obtained crystals are dissolved in an aqueous solution, and then separated by crystallization through one or more chromatographic resin columns to obtain vancomycin.

Embodiment 1

[0025] According to step a, the pH of the 2-picoline is 1.0; according to step b, by adding a water-miscible organic solvent to the precipitate to crystallize, the content of vancomycin in the solution before crystallization is 40%; the The organic solvent is methanol; the added amount of the organic solvent is: methanol is 2 times the volume of the crystallization solution; according to step b, the initial temperature of the crystallization process is 25°C; the end temperature of the crystallization process is 0°C; the cooling rate of the crystallization process is 2 °C / min; according to step c, the concentration of vancomycin after the crystals are dissolved in water is 60%.

Embodiment 2

[0027] According to step a, the pH of the 2-picoline is 2; according to step b, by adding a water-miscible organic solvent to the precipitate to crystallize, the content of vancomycin in the solution before crystallization is 50%; the The organic solvent is methanol; the added amount of the organic solvent is: methanol is 3 times the volume of the crystallization solution; according to step b, the initial temperature of the crystallization process is 35°C; the end temperature of the crystallization process is 10°C; the cooling rate of the crystallization process is 3 °C / min; according to step c, the concentration of vancomycin after the crystals are dissolved in water is 70%.

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Abstract

The invention discloses a preparation method for preparing vancomycin from 2-methylpyridine. The preparation method comprises the following steps: a, rapidly mixing an antibiotic fermentation mixture with 2-methylpyridine so as to obtain a solution with a pH value of at least about 7.8, and allowing the obtained solution to continue precipitation without stirring; b, crystallizing the precipitate formed in the step a from the solution; and c, dissolving the obtained crystal so as to obtain an aqueous solution, and carrying out crystallization separation through one or more resin chromatographic columns so as to obtain the vancomycin. The vancomycin prepared by using the preparation method provided by the invention has the following advantages: effective components are greatly improved; impurities are greatly reduced; the purity is high; the chromatographic purity can reach 95% or above; meanwhile, the vancomycin has significantly-improved appearance and color, and is applicable to oral or injection administration. The invention has the following advantages: the preparation method is simple and convenient; and the technological process is applicable to mass production.

Description

technical field [0001] The invention relates to the technical field of preparation methods of vancomycin, in particular to a preparation method of vancomycin by 2-picoline. Background technique [0002] Vancomycin is an antibiotic with the molecular formula C66H74Cl2N9O24. Its half-life: 4 to 8 hours, 9 days for renal failure, ineffective against anaerobic bacteria and Gram-negative bacteria, and will not be removed by hemodialysis. The "superbug" NDM-1 that appeared in India and other South Asian countries has spread to the United Kingdom, the United States, Canada, Australia, the Netherlands and other countries. Domestic experts say that the South Asian superbug will not become a pandemic, and vancomycin can be effective. [0003] Vancomycin belongs to glycopeptide macromolecular antibiotics. Vancomycin is more powerful and will be used when other antibiotics are ineffective against bacteria. It is mainly used for systemic and intestinal infections caused by Staphylococc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K9/00C07K1/30
Inventor 苗玉武吕祖平刘永刚王丹丹刘言华
Owner 江苏海阔生物医药有限公司
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