Method for finely purifying caspofungin

A caspofungin, fine technology, applied in the preparation method of peptides, chemical instruments and methods, organic chemistry, etc., can solve the problem that the purity of caspofungin does not meet the high The quality cannot be well separated and controlled, and the process is complicated, etc.

Inactive Publication Date: 2015-09-16
SUZHOU NANOMICRO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Therefore, the method for purifying caspofungin disclosed in the prior art has two deficiencies: one is that the purity of caspofungin does not meet the corresponding high-purity requirements, and even if it reaches the standard, the process is more complicated; Second, the amount of caspofungin single-component impurity cannot be well separated and controlled, such as making the single-component impurity less than 0.1%

Method used

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  • Method for finely purifying caspofungin
  • Method for finely purifying caspofungin
  • Method for finely purifying caspofungin

Examples

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Embodiment 1

[0020] by Finely purify caspofungin as a chromatographic medium: use a 15×310mm glass chromatographic column, (produced by Suzhou Nawei Technology Co., Ltd.) is a chromatographic column packed with chromatographic packing material, and the column volume is 55ml. 0.5 g of crude caspofungin (purity 91%) was dissolved in 8 ml of water, and filtered through a 0.45 μm filter membrane for later use. The above-mentioned caspofungin solution is loaded into the chromatographic column, washed with 21% aqueous acetonitrile (containing 0.03%-0.2% acetic acid) at 7ml / min for 12 column volumes (BV), and the eluted Caspofungin, through HPLC analysis, the peak area of ​​caspofungin in the eluent is 99.8% of the total area, the single-component impurity is less than 0.1%, and the recovery rate is 61.8%.

[0021] figure 1 It is the HPLC analysis spectrum of caspofungin crude product before purification. It can be seen that there are many impurities and the content is high. figure 2 It i...

Embodiment 2

[0023] by Finely purify caspofungin as a chromatographic medium: use a 15×310mm glass chromatographic column, (C18 reversed-phase silica gel filler, produced by Suzhou Nawei Technology Co., Ltd.) was used to fill the chromatography column with a packing volume of 55 ml. 0.5 g of crude caspofungin (purity 91%) was dissolved in 8 ml of water, and filtered through a 0.45 μm filter membrane for later use. Say above-mentioned caspofungin solution loads in the chromatographic column, wash 16 column volumes (BV) with 21% acetonitrile aqueous solution with 7ml / min, collect the caspofungin that is eluted, analyze through high performance liquid phase , the peak area of ​​caspofungin in the eluate is 97.6% of the total area, the single-component impurity is less than 0.15%, and the recovery rate is 60.2%.

Embodiment 3

[0025] by Finely purify caspofungin as a chromatographic medium: use a 15×310mm glass chromatographic column, (C18 reversed-phase silica gel filler, produced by Suzhou Nawei Technology Co., Ltd.) was used to fill the chromatography column with a packing volume of 55 ml. 0.5 g of crude caspofungin (purity 91%) was dissolved in 8 ml of water, and filtered through a 0.45 μm filter membrane for later use. Say above-mentioned caspofungin solution loads in the chromatographic column, wash 16 column volumes (BV) with 21% acetonitrile aqueous solution with 7ml / min, collect the caspofungin that is eluted, analyze through high performance liquid phase , the peak area of ​​caspofungin in the eluate is 96.5% of the total area, the single-component impurity is less than 0.15%, and the recovery rate is 60.9%.

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Abstract

The invention provides a method for finely purifying caspofungin, which comprises the following steps: by using monodisperse polymer 30BPC microspheres as a column chromatography filler, loading a caspofungin crude product solution onto the chromatographic column, eluting caspofungin adsorbed onto the filler by using a water solution and an organic solvent as mobile phases, and collecting the caspofungin-rich solution. By using the method, the caspofungin purity can reach 99% above, and the single-component impurity can be controlled at 0.1% below. The method has the advantages of simple process and high purification efficiency, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of drug purification, in particular to a method for purifying caspofungin, an echinocandin antifungal drug. Background technique [0002] Caspofungin is a macrocyclic lipopeptide from the echinocandin family, which can inhibit the synthesis of β-(1,3)-D-glucan in the cell wall of many filamentous fungi and yeast, destroying the integrity of the cell wall, and Produces a fungicidal effect. The structural formula of caspofungin is as follows: [0003] [0004] Caspofungin is a semi-synthetic derivative of pneumocandine B0 (neumocantine B0), which is synthesized from the fermentation product of Glarea Lozoyensis. The synthesized caspofungin must be separated and purified before reaching the purity of pharmaceutical standards. [0005] Impurities in drugs generally have no therapeutic effect, and some have certain toxicity, which is the main factor affecting the safety of drugs. The US Food and Drug Administration ...

Claims

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Application Information

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IPC IPC(8): C07K7/56C07K1/16
Inventor 江必旺吴俊成陈荣姬潘毅
Owner SUZHOU NANOMICRO TECH CO LTD
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