Method for separating and purifying caspofungin or its salt

A technology for crude caspofungin and salt, applied in peptide preparation methods, chemical instruments and methods, organic chemistry, etc., can solve the problem that product yield or purity cannot meet product quality and safety, and increase the production of caspofungin impurities , Unfavorable quality and safety control and other issues, to achieve the effect of easy operation of separation conditions, quality assurance, and reduced production costs

Inactive Publication Date: 2014-12-31
BRIGHTGENE BIO MEDICAL TECH (SUZHOU) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN102153616 discloses a method for separating and purifying caspofungin with perforated resins, but the products obtained by this method need to be recrystallized to obtain higher purity, so repeated separation and purification operations are often carried out above the refrigerated temperature It increases the possibility of caspofungin impurities, which is very detrimental to the quality and safety control of the final product
Not only does it increase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 5g of crude caspofungin and dissolve it in 400ml of 45% ethanol-water (V / V) solution, adjust the pH to 4.0 with formic acid, filter to obtain 400ml of filtrate, and apply the above-mentioned filtrate to a reversed-phase column.

[0026] Take 300g reverse-phase silica gel UniSil TM 20-RPC C18 filler with a pore size of 100 ?, use 95% ethanol solution to pack the column, the column shape is 300mm×15mm×5 um, and then use 35% by volume: 10% ethanol-formic acid The solution equilibrates the column. Under normal temperature and pressure, the speed of the mobile phase is 110mL / min. After loading the sample, wash with 1500ml of ethanol-methanol solution with a volume percentage of 45%:15%, and then use a volume percentage of 65%:10% ethanol-methanol solution 1500ml was analyzed, and the collection started after 1000ml was eluted, and the collection was stopped after a total of 1500ml was collected. The collected solution was combined and concentrated under reduced pressure...

Embodiment 2

[0029] Take 5g of crude caspofungin and dissolve it in 400ml of 45% ethanol-water (V / V) solution, adjust the pH to 4.0 with formic acid, filter to obtain 400ml of filtrate, and apply the above-mentioned filtrate to a reversed-phase column.

[0030] Take 300g reverse-phase silica gel UniSil TM 10-RPC C8 filler with a pore size of 100 ?, use 95% ethanol solution to pack the column, the column shape is 250mm×20mm×5 um, and then use 35% by volume: 10% ethanol-formic acid The solution equilibrates the column. At normal temperature and pressure, the mobile phase speed is 110mL / min. After loading the sample, wash with 1600ml of ethanol-methanol solution with a volume percentage of 40%:10%, and then use a volume percentage of 60%:10% ethanol-methanol solution 1500ml was analyzed, 1000ml was eluted and collected, and the collection was stopped after a total of 1500ml was collected. The collected solution was combined and concentrated under reduced pressure at 50°C to 500ml.

[0031] T...

Embodiment 3

[0033] Take 5g of crude caspofungin and dissolve it in 500ml of 45% ethanol-water (V / V) solution, adjust the pH to 4.0 with formic acid, filter to obtain 500ml of filtrate, and apply the above-mentioned filtrate to a reversed-phase column.

[0034] Take 300g reverse-phase silica gel UniSil TM 50-RPC C4 filler with a pore size of 100 ?, use 95% ethanol solution to pack the column, the column shape is 250mm×20mm×5 um, and then use 35% by volume: 10% ethanol-formic acid The solution equilibrates the column. Under normal temperature and pressure, the speed of the mobile phase is 110mL / min. After loading the sample, wash with 1500ml of ethanol-methanol solution with a volume percentage of 50%: 20%, and then use a volume percentage of 70%: 10% ethanol-methanol solution 1500ml was analyzed, 1000ml was eluted and collected, and the collection was stopped after a total of 1500ml was collected. The collected solution was combined and concentrated under reduced pressure at 50°C to 500ml....

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PUM

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Abstract

The invention provides a method for separating and purifying caspofungin or its salt, which comprises the following steps: separating caspofungin or its pharmaceutically acceptable salt in a reversed column chromatography, then recrystallizing, and drying to obtain caspofungin or its pharmaceutically acceptable salt with high purity. The prepared end product has the advantages of high purity and low production cost, the medicine quality is increased, operation is simple, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separation and purification of caspofungin or a pharmaceutically acceptable salt thereof. Background technique [0002] Caspofungin (Caspofungin) is a semi-synthetic derivative of pulmonary candidain B0 (neumocontin B0) with spectrum antifungal activity. Its acetate salt was first launched in the United States in February 2001. The structural formula of caspofungin is shown in formula I: [0003] [0004] Caspofungin is a semi-synthetic lipopeptide (echinocandin) compound synthesized from the fermentation product of Glarea Lozoyensis, and its preparation methods are disclosed in multiple patents such as WO9421677, EP620232, and WO9624613. After fermentation and semi-synthesis, caspofungin must be separated and purified to meet pharmaceutical standards. [0005] US5552521 discloses a method for purifying caspofungin by preparative HPLC, using a C18 column as a stationary phase and acetonitrile / water / acetic aci...

Claims

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Application Information

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IPC IPC(8): C07K7/56C07K1/20
Inventor 袁建栋
Owner BRIGHTGENE BIO MEDICAL TECH (SUZHOU) CO LTD
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