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Preparation method of caspofungin acetate impurity B

A technology of caspofungin acetate and impurities, which is applied in the field of chemistry and achieves the effects of high yield, satisfying requirements and stable conditions

Pending Publication Date: 2021-12-17
HANGZHOU ZHONGMEI HUADONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the prior art, there is no relevant report on how to prepare high-purity caspofungin acetate impurity B. Therefore, a method for preparing high-purity caspofungin acetate impurity B needs to be developed to meet the needs of the enterprise itself and the market. Need for Caspofungin Acetate Impurity B Reference Substance

Method used

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  • Preparation method of caspofungin acetate impurity B
  • Preparation method of caspofungin acetate impurity B
  • Preparation method of caspofungin acetate impurity B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] First, determine the aqueous phase, packing material, mobile phase, and elution gradient.

[0032] 1. Determination of the aqueous phase

[0033] First, 0.1% acidic water is used as the water phase, and acetonitrile is used as the mobile phase. Since the stability of super antibiotic products is generally not good, it is necessary to further investigate the stability of the product during the preparation process. Therefore, aqueous solutions with different acidities are used for preparation. The results are as follows Table 1 shows:

[0034] Table 1 Effect of different water relative to the purity of impurity B in the collected components

[0035]

[0036] As can be seen from the above experimental results, when 0.1% acetic acid aqueous solution is used, the purity of the prepared components of impurity B can reach 95%, and the effect is the best, so 0.1% acetic acid aqueous solution is determined as the water phase.

[0037] 2. Determination of filler

[0038] Ac...

Embodiment 2

[0051] According to the same method and chromatographic conditions as in Example 1, 4 g of crude product B with a purity (impurity B content) of 52% was dissolved in 0.1% acetic acid aqueous solution, and finally, impurity B in the collected gradient eluent and isocratic eluent The content is more than 95%, and the total yield of the product is 45%. The eluent collected is combined and freeze-dried to obtain a solid powder of 0.9g impurity B, such as figure 2 As shown in the detection spectrum, the product purity is 96.31%.

Embodiment 3

[0053] According to the same method and chromatographic conditions as in Example 1, 3 g of crude product B with a purity (impurity B content) of 52% was dissolved in 0.1% acetic acid aqueous solution. Finally, the collected gradient eluent and isocratic eluent contained impurities The content of B is more than 95%, and the total yield of the product is 41%. The eluent collected by merging is freeze-dried to obtain the solid powder of 0.6g impurity B, such as image 3 As shown in the detection spectrum, the product purity is 97.04%.

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Abstract

The invention relates to a method for preparing a caspofungin acetate impurity B. The method comprises the following steps of 1) preparing the caspofungin acetate impurity B crude product into a solution, and filtering; 2) separating and purifying the filtered crude product solution through a chromatographic column in a preparation system, and collecting an eluent; and 3) carrying out freeze drying on the qualified eluent to obtain caspofungin acetate impurity B solid powder with the purity of 95% or above. According to the method for preparing the chromatography, isocratic and gradient elution is carried out by adopting a mixed solution of 0.1% acetic acid and acetonitrile as a mobile phase, finally, impurity B solid powder with the purity larger than 95% is obtained, so that the preparation method of the high-purity caspofungin acetate impurity B is provided, and the requirements of enterprises and markets can be met; and the preparation method is stable in condition, suitable for large-scale production and high in yield.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a preparation method of caspofungin acetate impurity B. Background technique [0002] Caspofungin acetate is the first echinocandin antifungal drug, which was approved by the US FDA in 2001. It is mainly used for the treatment of invasive candidiasis and invasive aspergillosis that is ineffective or intolerable to other treatments And empiric treatment of neutropenia and suspected fungal infection in patients with fever. As a representative of a new class of echinocandin antibiotics, caspofungin acetate has high selectivity, good antibacterial activity, and high safety. The obvious advantage in terms of less drug resistance. [0003] Caspofungin acetate is firstly fermented by Glarea Lozoyensis to obtain the fermentation product, and then the fermented product undergoes solid-liquid separation, leaching, adsorption analysis, concentration and drying to obtain the crude produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/56C07K1/20C07K1/34C07K1/36
CPCC07K7/56
Inventor 周陈锋施林峰朱益新陈辅辰蔡鹭谢厅
Owner HANGZHOU ZHONGMEI HUADONG PHARMA