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Sulfate polymyxin B crystal and preparation method thereof

A technology of polymyxin sulfate and polymyxin, applied in the direction of preparation methods of polymyxin and peptides, chemical instruments and methods, etc., can solve the problems of crystallized precipitates that are easy to stick into agglomerates, clarity and purity Advanced problems, to achieve the effect suitable for large-scale industrial production, good clarity and purity, low hygroscopicity

Pending Publication Date: 2018-03-06
HUBEI RUIHAO ANKE MEDICINE TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems in the prior art that the clarity and purity of polymyxin B sulfate products are not high, and crystal precipitates are easily bonded into agglomerates, the invention provides a polymyxin B sulfate crystal and a preparation method thereof

Method used

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  • Sulfate polymyxin B crystal and preparation method thereof
  • Sulfate polymyxin B crystal and preparation method thereof
  • Sulfate polymyxin B crystal and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Take 5L of polymyxin B fermented liquid, the potency is 1.8g / L, add oxalic acid solid to adjust the pH to 1.8. After stirring for 30 minutes, add 250g of diatomaceous earth, continue to stir for 30 minutes, then filter with a plate frame, wash with water until the titer is less than 0.2g / L, stop filtering, and obtain 7.1L of filtrate, which contains 8.5g of polymyxa Prime B. The filtrate was adjusted to pH 6.7 with 2M sodium hydroxide, then loaded into a chromatographic column containing 60 ml of LXD-135 weakly acidic ion exchange resin, and adsorbed through the column. After adsorption is complete, adopt the water washing of 2-3 times volume by the volume meter of LXD-135 weakly acidic ion-exchange resin until the effluent is colorless, then desorb with 0.2M sulfuric acid aqueous solution, obtain desorption liquid 800ml (containing polymyxa sulfate Vitamin B 7.4g). The pH of the desorbed solution was adjusted to 6.5 with 2M sodium hydroxide solution, and then loaded ...

Embodiment 2

[0049] Get polymyxin B fermented liquid 5L, titer is 1.8g / L, then prepare desorption liquid according to the technique of embodiment 1. The desorbed solution obtained in this embodiment is a concentrated solution with a volume of 50 ml (containing polymyxin B sulfate 5.3 g) after concentration. Start stirring, and slowly add ethyl acetate dropwise to the concentrated solution until the solution becomes turbid, then stop adding ethyl acetate dropwise. Then lower the temperature to 0-5°C, stir until the solid precipitates, and then continue to add the remaining ethyl acetate dropwise until a total of 3 times the amount of ethyl acetate based on the volume of the concentrated solution is added dropwise. Stirring was then continued at 0-5°C for 7 hours, and the solid was filtered off. The filtered solid was vacuum-dried at 60°C for 3 hours to obtain 4.82g of a white solid, with a crystallization yield of 91%, a purity of 89.58%, a clarity test result of No. 1, and a titer of 8355...

Embodiment 3

[0051] Get polymyxin B fermented liquid 7L, titer is 1.8g / L, then prepare desorption liquid according to the technique of embodiment 1. The desorbed solution in this example was concentrated to obtain a concentrated solution (containing polymyxin B sulfate 6.7 g) with a volume of 85 ml. Start stirring, and slowly drop acetone into the concentrated solution until the solution becomes turbid, then stop adding acetone. Then lower the temperature to 0-5° C., stir until the solid precipitates, and then continue to drop the remaining acetone until a total of 3.5 times the amount of acetone based on the volume of the concentrated solution is added dropwise. Then continue stirring at 0-5°C for 6 hours, filter the solid, and dry the filtered solid in vacuum at 60°C for 4 hours to obtain 5.83g of white solid with a crystallization yield of 87%, a purity of 90.98%, and a clear Degree No. 1, the potency determined by the tube-and-dish method is 8100U / g. Under the same conditions, the cr...

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Abstract

The invention provides a sulfate polymyxin B crystal and a preparation method thereof. The preparation method comprises the following steps: firstly, adsorbing polymyxin B fermented liquid with resin,and adding a sulfate aqueous solution and / or an acid ethanol aqueous solution for desorption to obtain a desorption solution; secondly, adjusting a pH value of the desorption solution obtained in thefirst step to 5.0 to 7.0; and then concentrating until a solid is precipitated to obtain a sulfate polymyxin B saturated solution; and thirdly, in a stirring state, dropwise adding an organic solventinto the sulfate polymyxin B saturated solution obtained in the second step or dropwise adding the sulfate polymyxin B saturated solution obtained in the second step into the organic solvent so as toseparate out the crystal, filtering and drying a filter cake, thus obtaining the sulfate polymyxin B crystal. The solvent used in the preparation method disclosed by the invention is low in cost andeasy to obtain; the preparation method disclosed by the invention is suitable for large-scale industrial production; and the prepared sulfate polymyxin B crystal product has the advantages of higher purity and clarity and low moisture absorption.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a polymyxin B sulfate crystal and a preparation method thereof. Background technique [0002] Polymyxin B is a basic cyclic polypeptide antibiotic composed of various amino acids and fatty acids produced by Bacillus polymyxa. Polymyxin B products are multi-component mixtures, including polymyxin B1, B2, B3, and B1-1 (the sum of the mass of these four components is required by the European Pharmacopoeia to be ≥80.0%), and its sulfate is commonly used in clinical practice. . Polymyxin B sulfate is white or off-white powder with hygroscopicity. Polymyxin B sulfate has a strong killing effect on Gram-negative bacteria, especially NDM-1 bacteria (super bacteria), which has a high in vitro sensitivity, so it has attracted much attention. [0003] For the refining of polymyxin B sulfate finished product, because it is not easy to crystallize, spray drying method (patent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/62C07K1/36C07K1/30C07K1/22C07K1/18C07K1/107A61K38/12A61P31/04
CPCA61K38/00C07K7/62C07K2299/00
Inventor 王增霞李小兵罗汾李长洪许彦伟陈龙
Owner HUBEI RUIHAO ANKE MEDICINE TECH DEV CO LTD
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