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Crystallization of polymyxin sulfate b1, b2 or mixture thereof and preparation method thereof

A polymyxin sulfate and crystallization technology, which is applied to the crystallization of polymyxin sulfate B1, B2 or their mixtures and the field of their preparation, can solve the problem that the products are easy to stick to form agglomerates, affect the quality and curative effect of drugs, production and research. Inconvenience and other problems, to achieve the effect of improving drug quality and loosening crystal particles

Active Publication Date: 2020-12-04
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

However, the polymyxin B sulfate prepared by the current spray-drying method is difficult to form a crystal form, and the product is easily bonded into agglomerates, which brings a lot of inconvenience to production and research, and also affects the quality and efficacy of the drug

Method used

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  • Crystallization of polymyxin sulfate b1, b2 or mixture thereof and preparation method thereof
  • Crystallization of polymyxin sulfate b1, b2 or mixture thereof and preparation method thereof
  • Crystallization of polymyxin sulfate b1, b2 or mixture thereof and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Ethanol-water system: Take 100ml of polymyxin B1 sulfate aqueous solution with a concentration of 50g / L, stir at room temperature, add 3 times the volume of 95% (v / v) ethanol aqueous solution, and polymyxin B1 sulfate crystallizes out. After stirring at a temperature of 0-5° C. for 3-5 hours, filter, and vacuum-dry for 8 hours to obtain crystalline polymyxin sulfate B1, the crystal form is crystal form A.

Embodiment 2

[0068] Isopropanol-water: Take 26ml of polymyxin sulfate B1 and B2 aqueous solutions with a concentration of 50g / L, and slowly add it dropwise to 260ml (10 times the volume) of isopropanol under stirring. The temperature of isopropanol is always Control at 5-10°C. The crystals of polymyxin sulfate B1 and B2 precipitated during the dropwise addition gradually increased and were in a state of uniform dispersion without adhesion. Stirring was continued for 1 hour, the solid was obtained by filtration, and vacuum-dried for 10 hours to obtain 1.23 g of polymyxin sulfate B1 and B2 crystalline powders with a crystallization yield of 94.6%, wherein the crystal form of polymyxin sulfate B1 was crystal form 1.

Embodiment 3

[0070] n-Butanol-Water: Take 13.5g of polymyxin B2 sulfate, dissolve it in 150ml of pure water, and slowly add it dropwise to 1500ml (10 times the volume) of n-butanol in a stirring state, the temperature is always controlled at 25-30°C. During the dropping process, the precipitated polymyxin B2 sulfate gradually increased, and it was in a state of uniform dispersion, no adhesion, and good granularity. After the polymyxin B2 sulfate aqueous solution was added dropwise, the stirring was continued for 30 min, filtered, and vacuum-dried for 20 hours to obtain 13.2 g of polymyxin B2 sulfate crystalline powder with a crystallization yield of 97.8%.

[0071] From the XRD patterns of polymyxin B2 sulfate and polymyxin B1 sulfate, it can be seen that in the XRD pattern of polymyxin B2 sulfate, there is a weak small peak at 2θ=31.8°.

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Abstract

The invention provides an anhydride crystal of polymyxin sulfate B1, B2 or mixture thereof as well as a preparation method of the crystal. The preparation method comprises the following steps: (1) adding water into the polymyxin sulfate B1, B2 or the mixture thereof to enable the solid to be completely dissolved to obtain a saturated solution; (2) adding an organic solvent into the saturated solution slowly and dropwise, or adding the saturated solution into the organic solvent slowly and dropwise, separating out the solid and controlling the temperature of the dropwise adding process to be within the range of 0 to 60 DEG C, wherein the organic solvent is selected from one or more of C1-C4 alcohol, C3-C4 ketone or ethyl acetate, and butyl acetate; (3) filtering out the solid and vacuum-drying to obtain the anhydride crystal of the polymyxin sulfate B1, B2 or the mixture thereof, wherein the polymyxin sulfate B1 has a crystal form 1 and a crystal form A. The anhydride crystal particlesof the polymyxin sulfate B1, B2 or the mixture thereof, prepared by the method, are loose, non-sticky and particularly favorable for industrialized production of medicine products. In addition, by themethod, impurities in the medicines can be effectively removed, higher purity and clarity are achieved, and the quality of the medicine products is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to the crystallization of polymyxin sulfate B1, B2 or a mixture thereof 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 compounds, including polymyxin B1, B2, B3, and B1-1 (the sum of the four components required by the European Pharmacopoeia is ≥80.0%), and its sulfate salt is commonly used, which is white or Off-white powder, hygroscopic. 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. Because the two components of polymyxin B3 and B1-1 have nephrotoxicity, the mixture containing four components is mainly used externally clinically. The...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/62C07K1/30A61K38/12A61P31/04
CPCA61K38/00C07K7/62C07K2299/00Y02A50/30
Inventor 李小兵罗汾王增霞许彦伟李长洪
Owner HUBEI RUIHAO ANKE MEDICINE TECH DEV CO LTD
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