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Partricin A separation method
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A separation method and the technology of paltroxine, which are applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., to achieve the effects of stable product quality, simple operation, and low cost
Inactive Publication Date: 2015-03-04
SHANGHAI INST OF PHARMA IND CO LTD
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Abstract
Description
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Problems solved by technology
[0005] The technical problem to be solved by the present invention is to overcome that the existing method for separating patroxacin A uses a large amount of solvent to cause great pressure to the environment, and it is unavoidable to use activated carbon in the steps, and the unstable adsorption performance of activated carbon will cause the final product to be damaged. The defect of unstable quality provides a method for the separation of patraxacin A that is simple to operate, low in cost, does not produce too much solvent and causes environmental pressure, and has stable product quality and is suitable for large-scale industrial production.
Method used
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Effect test
Embodiment 1
[0065] Adjust the pH of the fermented broth containing patrixacin A 543 μg / mL obtained by fermentation to 3.0 with oxalic acid, let it stand for 2 hours and then filter it with suction, soak the filter cake in 2 times the volume of methanol for 2 hours, filter the filtrate after soaking, and filter the filter cake Repeat the operation once, and combine the two filtrates.
[0066] Adjust the pH of the filtrate to 9.0, and slowly concentrate at 30°C to a water content of 33%. At this time, a certain amount of solids precipitated, and then placed in a refrigerator at 4°C for 24 hours to fully precipitate patraxacin from the mother liquor, and suction filtered the precipitates After collection, it was dissolved with methanol solution containing 25% water, and passed through NM100 resin. After adsorption, it was pre-washed with 3CV methanol solution containing 20% water to remove impurities, and then patraxacin A was eluted with methanol solution containing 15% water. Patroxacin ...
Embodiment 2
[0069] Use oxalic acid to adjust the pH of the fermented fermented broth containing patrixacin A 528 μg / ml to 3.0, let it stand for 2 hours and then filter it with suction, soak the filter cake in 2 times the volume of acetone for 2 hours, filter the filtrate after soaking, and filter the filter cake Repeat the operation once, and combine the two filtrates.
[0070] Adjust the pH of the filtrate to 9.0, and slowly concentrate at 30°C to a water content of 33%. At this time, a certain amount of solids precipitated, and then placed in a refrigerator at 4°C for 24 hours to fully precipitate patraxacin from the mother liquor, and suction filtered the precipitates After collection, it was dissolved with methanol solution containing 25% water, and passed through NM100 resin. After adsorption, it was pre-washed with 3CV methanol solution containing 20% water to remove impurities, and then patraxacin A was eluted with methanol solution containing 15% water. Patroxacin A with a purit...
Embodiment 3
[0073] Adjust the pH of the fermented broth containing 501 μg / mL patrixacin A obtained by fermentation to 3.0 with oxalic acid, suction filter after standing for 2 hours, soak the filter cake with 2 times the volume of absolute ethanol for 2 hours, filter the filtrate after soaking, and The filter cake operation was repeated once, and the two filtrates were combined.
[0074] Adjust the pH of the filtrate to 9.0, and slowly concentrate at 30°C to a water content of 33%. At this time, a certain amount of solids precipitated, and then placed in a refrigerator at 4°C for 24 hours to fully precipitate patraxacin from the mother liquor, and suction filtered the precipitates After collection, it was dissolved with methanol solution containing 25% water, and passed through NM100 resin. After adsorption, it was pre-washed with 3CV methanol solution containing 20% water to remove impurities, and then patraxacin A was eluted with methanol solution containing 15% water. Patroxacin A wi...
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Abstract
The invention discloses a partricin A separation method, which comprises the following steps of: adjusting pH of a partricin-containing fermentation broth, standing and filtering, immersing the filter cake by a polarity organic solvent, filtering and taking a filtrate; adjusting pH of the filtrate, condensing at the temperature of 25-35 DEG C until the water content is 30-35%, standing and filtering to obtain a partricin crude product; dissolving the crude product in a methanol solution containing 25-30% of water, loading the solution into a styrene macroporous anti-phase adsorption resin column, carrying out elution and removing impurities by using a methanol solution containing 18-23% of water, carrying out elution on partricin A by using a methanol solution containing 13-17% of water, collecting a partricin A eluate with the purity being greater than or equal to 80%, condensing the collected partricin A eluate to a methanol solution containing 25-30% of water, loading to the column, carrying out elution and removing impurities by using a methanol solution containing 17-19% of water, carrying out elution by using a methanol solution containing 10-14% of water, and collecting the eluate, wherein the percentage is volume percentage. The method provided by the invention has advantages of simple operation, low cost, little solvent and stable product quality, and is suitable for large-scale industrial production. The purity of the separated product partricin A reaches more than 93%.
Description
technical field [0001] The invention relates to a method for separating patroxine A. Background technique [0002] In 1971, Tiberio Bruzzese et al. isolated and purified a strain of Streptomyces aureofaciens from soil samples, and isolated a heptacene macrolide antibiotic from the metabolites of the bacterium, named It is partricin. Patroxacin is a high-efficiency antifungal and antiprotozoal drug, which achieves antibacterial effect by inhibiting the synthesis of fungal cell membranes, especially has extremely high antibacterial activity against Candida albicans. Patroxine mainly contains two components, patroxine A and patroxine B. [0003] In the fermentation product of Streptomyces aureus, in addition to the product patraxacin, a large amount of tetracycline, aureomycin and other antibiotics and impurities are also produced at the same time. . At present, the separation and purification of patroxacin A in the prior art mainly adopts traditional methods such as organi...
Claims
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Application Information
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