Preparation method of impurities B1, B2, B3 and B1-1 in polymyxin B sulfate

Through the low-pressure chromatography system combined with the separation and purification process of analyzing pure solvents, the separation and purification problem of the main components and impurities in polymyxin sulfate B was solved, and the preparation of high-purity products was realized, the process was simplified, the cost was reduced, and it was suitable for large-scale production.

CN119735648APending Publication Date: 2025-04-01SHENZHEN HUAYAO NANFANG PHARM CO LTD
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Patent Information

Application Number
CN202510114041.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-24
Publication Date
2025-04-01

AI Technical Summary

Technical Problem

The prior art is difficult to efficiently separate and purify the main components B1, B2 and main impurities B3, B1-1 in polymyxin sulfate B, making it difficult for the product quality to meet the pharmacopoeia standards. The existing methods are costly, have low yields and high equipment requirements, making it difficult to meet the needs of large-scale preparation.

Method used

A low-pressure chromatography system was used to combine C18 filler, acetonitrile, dipotassium hydrogen phosphate, ammonia water and other analyses pure solvents, and through specific separation and purification, concentration desalination, crystallization or lyophilization processes, high-purity B1, B2, B3 and B1-1 were successfully prepared.

Benefits of technology

The preparation of high purity B1, B2, B3 and B1-1 is achieved, and the product purity can reach 96.05%, 91.28%, 94.83%, etc., simplifying the preparation process, reducing costs and equipment requirements, and is suitable for large-scale production.

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Abstract

The invention provides a preparation method of impurities B1, B2, B3 and B1-1 in polymyxin sulfate B. The method comprises the following steps: preparing raw materials: taking polymyxin sulfate B as a raw material, using 30-50m C18 as a filler, acetonitrile, dipotassium hydrogen phosphate, ammonia water, anhydrous sodium sulfate, phosphoric acid and trifluoroacetic acid as analytically pure materials, using deionized water, and using a nylon column as a column; conducting analytical purification: weighing raw materials and adding fillers into the column, loading the sample, and treating the sample with an eluent; conducting concentration and desalting on the analytically purified fraction; conducting concentration and desalting on the fraction in step 3; conducting crystallization: reducing the pressure on the fraction in step 3 to recover the solvent on a rotary evaporator, adding ammonia water to adjust the pH value to precipitate the precipitate, filtering, washing with water, and vacuum drying to obtain the product; and successfully preparing high-purity B1, B2, B3 and B1-1 through a specific process combination of separation and purification, concentration and desalting, crystallization or freeze drying. For example, the purity of B1 product can reach 96.05%, the purity of B3 can reach 91.28%, and the purity of B1-1 can reach 94.83%. These high-purity products, whether used as drug raw materials or scientific research reference substances, can provide a reliable material basis for related research and production, effectively reduce the interference of impurities on experimental and production results, and improve the accuracy of research and the stability of product quality.
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Citation Information

Patent Citations

  • Preparing method of high-purity polymyxin B

    CN103130876B

  • Preparation method of polymyxin B2

    CN115746101A