Purification method of echinocandins antifungal drug anidulafungin

Anidungin and antifungal technology are applied in the field of purification of echinocandin-type antifungal anidungin, which can solve the problems of long purification and separation time, difficult post-processing, few samples to be processed, etc. The effect of short separation time, low equipment cost and convenient operation

Active Publication Date: 2013-07-10
NCPC NEW DRUG RES & DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the equipment used in this method is expensive, the number of samples to be processed is small, the time for purification and separation is long, and post-processing is difficult, and the development cost is high. At present, it is still impossible to realize industrial scale-up production

Method used

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  • Purification method of echinocandins antifungal drug anidulafungin
  • Purification method of echinocandins antifungal drug anidulafungin
  • Purification method of echinocandins antifungal drug anidulafungin

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Take 22.5g of the crude product of Anifungin, add methanol to make it fully dissolve, then add 45g of amorphous silica gel (200-300 mesh) and stir evenly, and obtain a dry sample of Anidulungin silica gel after drying.

[0035] Pack 565g of amorphous silica gel (200-300 mesh) in a chromatographic column with a height-to-diameter ratio of 8:1, fill the dry sample of anifungin silica gel evenly on the top of the chromatographic column, and then use dichloromethane-methanol The mixed solution is used as the elution solvent for gradient pressure elution. The volume ratio of dichloromethane to methanol in the first gradient elution solvent is 90:10, and the volume ratio of dichloromethane to methanol in the second gradient elution solvent is 80. :20, the column pressure in the chromatographic column is 5bar. According to the monitoring result of high-performance liquid chromatography, collect the eluent with anifungin content greater than 98%. The amounts of the first gradi...

Embodiment 2

[0039] Take 20.5 g of crude anifungin, add tetrahydrofuran to dissolve it fully, then add 20.5 g of spherical silica gel (300 mesh to 400 mesh) and stir evenly, and dry it to obtain a dry sample of anidulungin silica gel.

[0040] Fill 410g of spherical silica gel (300 mesh to 400 mesh) in a chromatographic column with a height-to-diameter ratio of 9:1, fill the dry sample of anifungin silica gel evenly on the top of the chromatographic column, and then use a tetrahydrofuran-methanol mixed solution as the The elution solvent is subjected to gradient pressure elution, the volume ratio of tetrahydrofuran and methanol in the first gradient elution solvent is 90:10, and the volume ratio of tetrahydrofuran and methanol in the second gradient elution solvent is 75:25. The column pressure is 6bar. According to the monitoring result of high-performance liquid chromatography, collect the eluent with anifungin content greater than 98%. The amounts of the first gradient elution solvent ...

Embodiment 3

[0044] Take 15.2 g of the crude product of Anifungin, add dichloromethane-methanol to fully dissolve it, then add 45.6 g of amorphous silica gel (100 mesh to 200 mesh) and stir evenly, and dry it to obtain a dry sample of Anidifungin silica gel.

[0045] Fill 456g of amorphous silica gel (100 mesh to 200 mesh) in a chromatographic column with a height-to-diameter ratio of 12:1, fill the dry sample of anifungin silica gel evenly on the top of the chromatographic column, and then use a chloroform-methanol mixed solution Gradient pressure elution is carried out as the elution solvent, the volume ratio of chloroform and methanol in the first gradient elution solvent is 90:10, the volume ratio of chloroform and methanol in the second gradient elution solvent is 70:30, and the chromatography column The column pressure inside is 2 bar. According to the monitoring result of high-performance liquid chromatography, collect the eluent with anifungin content greater than 98%. The amounts...

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Abstract

The invention discloses a purification method of echinocandins antifungal drug anidulafungi. The method comprises the following steps of: (1) preparing a dry sample: adding organic solvent in a crude product of the anidulafungin to dissolve the crude product, adding silica gel after the crude product of the anidulafungin is adequately dissolved, and uniformly mixing and drying the mixture to obtain the anidulafungin dry sample; (2) pressurizing and eluting: uniformly filling the anidulafungin dry samples in the top end of a chromatographic column with silica gel, pressurizing and eluting the chromatographic column with the anidulafungin dry samples by adding elution solvent, utilizing a high-effective liquid phase chromatography to monitor, and collecting the elution solution with the anidulafungin content being greater than 98 percent; and (3) concentrating: concentrating the elution solution with the anidulafungin content being greater than 98 percent until dryness to obtain a pure product with the anidulafungin content being greater than 98 percent. By adopting the column chromatography, simplicity in operation is realized, and the equipment cost is low; the organic solvent with low toxicity and low boiling point is adopted as the elution solution, so that the subsequent recycling treatment is simple, and the environmental pressure can be greatly reduced; and the purification separation time is short, the purification effect is good, the purification yield is high, and the purification method is applicable to industrialized mass production.

Description

technical field [0001] The invention relates to a method for purifying an echinocandin antifungal drug anidifungin, which belongs to the technical field of drug synthesis and purification. Background technique [0002] In recent years, due to the extensive use of immunosuppressants caused by organ transplantation, the application of chemotherapy and more aggressive medical methods, the spread of AIDS, and the abuse of broad-spectrum antibacterial drugs, the number of people with suppressed immune systems has continued to increase. The incidence of infection has increased significantly, especially the incidence and mortality of deep fungal infections have increased year by year. At the same time, with the use of antifungal drugs, the drug resistance of fungi is becoming stronger and stronger, making the application of antifungal drugs have a trend of rapid increase. Therefore, anti-deep fungal infection drugs have become one of the research hotspots of anti-infective drugs a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/56C07K1/16
Inventor 邢振堂闫国婷陈峰孟国彬胡军平朱秀良吕彦超王芹芳张炜
Owner NCPC NEW DRUG RES & DEV
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