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Purification method of teicoplanin

A purification method and technology for teicoplanin, applied in the field of purification for separation of teicoplanin, can solve the problems of difficult crystallization and small change range, and achieve the improvement of effective components, the improvement of appearance and color, and the reduction of other impurities. Effect

Active Publication Date: 2009-05-06
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the solubility of teicoplanin does not vary greatly with temperature, so it is difficult to crystallize it by changing the temperature

Method used

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  • Purification method of teicoplanin
  • Purification method of teicoplanin
  • Purification method of teicoplanin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Teicoplanin fermentation broth 100L, potency 1268μg / ml, containing 126.8g teicoplanin, adjusted pH to 9.5 with 1M NaOH, filtered into ceramic membrane, the pore size of ceramic membrane is 0.02μm. After filtration and top washing with water, 110 L of mixed filtrate was obtained, with a titer of 928 μg / ml, containing 102.08 g of teicoplanin. The macroporous adsorption resin on the filtrate is adsorbed, the volume of the resin is 4L, and the flow rate is 10L / hr. After washing the resin with water, after washing 6 times the column volume, elute with an aqueous solution containing 60% acetone and pH 3.5 at a flow rate of 8 L / hr to obtain 3.8 L of eluent with a titer of 14105 μg / hr. ml, pH6.9, containing 53.599g of teicoplanin. After adjusting the pH to 5.0 with 1M HCl, add 50 g of activated carbon to the eluate, stir for 30 minutes, and filter to obtain 3.7 L of decolorized solution with a titer of 12680 μg / ml, pH 4.8, and 46.916 g of teicoplanin. The decolorization solut...

Embodiment 2

[0038] The concentration of the concentrated aqueous solution of teicoplanin obtained according to the method of Example 1 was 52000 μg / ml, the HPLC peak area ratio of the active ingredient was 75.8%, the HPLC peak area ratio of other impurities was 9.2%, the volume was 200ml, and the pH=8.2. After filtering through a 1 μm filter element, add 1M HCl solution while stirring to adjust the pH of the solution until the pH is stable at 2.5, from which teicoplanin is precipitated to form a suspension. After continuing to stir for 30 minutes, stop stirring, let stand for 12 hours, and control the process temperature at about 5°C. The mixture was filtered, and finally 50 ml of water was top-washed with pH=2.5 and temperature 0° C., and 18.6 g of wet crude product of teicoplanin was obtained after top-washing. The HPLC peak area ratio of the effective component of teicoplanin obtained by precipitation was 83.6%, and the HPLC peak area ratio of other impurities was 4.2%, and the appeara...

Embodiment 3

[0040] The concentration of the concentrated aqueous solution of teicoplanin obtained according to the method of Example 1 is 52000 μg / ml, and the effective component HPLC peak area ratio is 75.8% (, other impurity HPLC peak area ratios are 9.2%, volume 200ml, pH=8.2. By 1 μm Add 1M HCl solution while stirring to adjust the pH of the solution until the pH is stable at 2.5, and teicoplanin is precipitated therefrom to form a suspension. Continue to stir for 60 minutes and then stop stirring, let stand for 24 hours, process temperature control At about 15°C. The mixture is filtered, and finally 50ml of water with a pH of 2.5 and a temperature of 10°C is used for top washing, and 18.2g of wet crude product of teicoplanin is obtained after the top washing. The effective group of teicoplanin obtained by precipitation Part HPLC peak area ratio is 84.7%, other impurity HPLC peak area ratio is 4.0%, product outward appearance color obtains obvious improvement simultaneously.See Table 1...

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Abstract

The invention relates to a method for preparing glycopeptides antibiotic teicoplanin, which comprises the following steps: after teicoplanin fermented solution is subjected to filtration, adsorption by macroporous resin and decoloring by active carbon, the decoloring solution is concentrated and desolventizing by nanofilteration or hyperfiltration to obtain the teicoplanin water solution with high concentration, and then the teicoplanin is deposited from the solution by adjusting pH, adding salt or adjusting pH and adding salt simultaneously, and the mixture is filtered to obtain teicoplanin. The effective ingredients of the teicoplanin obtained through deposition are obviously improved, and other impurities are reduced. Meanwhile, the appearance color of the product is improved obviously.

Description

technical field [0001] The invention relates to a purification method for separating glycopeptide antibiotic teicoplanin, in particular to a purification method for separating teicoplanin from 2-20W / V% teicoplanin aqueous solution. Background technique [0002] Among the process patents for the preparation of teicoplanin that exist today, the preparation process is mainly to filter the fermentation broth after alkalization, and then desorb the resin with a desorbent after the filtrate is adsorbed by the resin. Precipitate and filter to obtain the wet product of teicoplanin. Then use resin or chromatographic agent for further refining, wherein the resin is mainly macroporous adsorption resin, the desorbent is an aqueous solution of organic solvent, and finally add a large amount of solvent for precipitation. [0003] The above method has been fully applied in specific production, and the effect is proved to be good. But the biggest problem is that the final precipitation st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K9/00C07K1/36C07K1/34C07K1/16
Inventor 卢伟良王小勇章槐东孙新强
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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