Method for separating and purifying method of polymyxin E methanesulfonic sodium

A technology for separation and purification of polymyxin, applied in the direction of peptides, anti-infectives, drug combinations, etc., can solve problems such as troublesome production process, increased cost, environmental burden, etc., and achieve complete reaction, easy control and amplification, and low energy consumption Effect

Active Publication Date: 2009-09-09
SHANGHAI INST OF PHARMA IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to use two kinds of chromatographic media, the production process is relatively cumbersome, and a large amount of ac

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take by weighing 80g (about 0.057mol) polymyxin E sulfate (product batch number is 20061001, its quality meets European Pharmacopoeia standard, wherein polymyxin E 1 and E 2The content is 71%), add water to dissolve and set the volume to 400ml, then add 49.6ml (about 0.661mol) of formaldehyde solution, stir and adjust the pH to 7 with 10mol / L NaOH solution, after maintaining the reaction for 30min, add 224ml (about 0.661mol) to it 0.862mol) 40% sodium bisulfite solution, and then adjust the pH to 7 with NaOH solution, and stop the reaction after reacting for 10 h under stirring. Get this reaction solution, use the ultrafiltration membrane that molecular weight cut off is 3000 (be the product of American MILLIPORE company, be the cellulose acetate membrane) ultrafiltration to about 130ml, then add water to about 675ml, then ultrafiltration concentrates to 130ml, so repeat 5 times, about 135ml of ultrafiltration retentate was obtained. The temperature was controlled at ...

Embodiment 2

[0024] Change the reaction time after adding formaldehyde in embodiment 1, make reaction time increase to 90 minutes, all the other operations are with embodiment 1, have obtained the polymyxin E methanesulfonic acid that does not contain sulfate radical and free polymyxin E The sodium product has a yield of 78%, and a product titer of 449 μg / mg.

Embodiment 3

[0026] Change the reaction time after adding sodium bisulfite in embodiment 1, make reaction time increase to 20 hours, all the other operations are with embodiment 1, have obtained the polymyxin that does not contain sulfate radical and free polymyxin E equally E sodium methanesulfonate product, the yield is 82%, and the product potency is 452 μ g / mg.

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Abstract

The invention relates to a method for separating and purifying polymyxin E methanesulfonic sodium from a mixture containing small-molecular weight impurities. The method adopts an ultrafiltration membrane with the cutoff molecular weight ranging from 1,000 to 10,000 to carry out separation and purification. The invention also relates to a method used for preparing high-purity E methanesulfonic sodium by controlling reaction conditions and making use of ultrafiltration membrane separation technology. The method comprises the following steps: (a) adding water to dissolve polymyxin E sulfate andthen adding formaldehyde solution in the solution to carry out reaction; (b) adding sodium bisulfite solution in the reaction products of step (a) to carry out reaction continuously; and (c) taking the reaction solution of step (b) and adopting the ultrafiltration membrane to carry out separation and purification. The method of separating and purifying the polymyxin E methanesulfonic sodium has the advantages of low pollution, low energy consumption, simple process, good repeatability and high purity and activity of obtained products.

Description

technical field [0001] The present invention relates to a method for separating and purifying polymyxin E sodium methanesulfonate, in particular to a method for separating and purifying polymyxin E sodium methanesulfonate from a mixture containing small molecular weight impurities using membrane separation technology, In addition, it also relates to a method for preparing high-purity polymyxin E sodium methanesulfonate by controlling reaction conditions and using membrane separation technology. Background technique [0002] Polymyxin E (colistin) is a polypeptide antibiotic composed of multiple components, mainly composed of E 1 and E 2 Composition (or called A or B). In the 1950s, polymyxin E was used clinically, mainly for the treatment of infections caused by Gram-negative bacteria, especially infections caused by multidrug-resistant Pseudomonas aeruginosa. There are two types of colistin used clinically, one is polymyxin E sulfate (also known as colistin sulfate) for ...

Claims

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Application Information

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IPC IPC(8): C07K7/64C07K7/06A61P31/00
Inventor 冯军张喜全朱裕辉张来芳赵伟薛春佳程艳菊胡博新
Owner SHANGHAI INST OF PHARMA IND
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