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
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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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