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Extraction and refinement of lovastatin

A technology of lovastatin and refining method, which is applied in the field of extracting and purifying lovastatin, which can solve the problems of using too many solvents, multiple extractions, and low extraction yield, and achieve the effects of reducing dosage, reducing environmental pressure, and reducing pressure

Inactive Publication Date: 2005-02-23
SHANDONG LUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are disadvantages in this method: too many solvents are used, and mixed solvents are used, which brings certain difficulties to solvent recovery
Unfortunately, this method still has some disadvantages: the extraction yield is low, multiple extractions are required, and the amount of dissolved coal is too large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Fermentation broth 10L, unit 7653u / ml, adjust to PH10 with 2mol / l NaOH, filter, add alkaline water continuously during the filtering process, stop filtering when the unit of the filtrate is lower than 200u / ml, collect the filtrate, and use the resin to adsorb the filtrate , desorbed with ethanol after adsorption. The desorption solution was concentrated in vacuum, 3.0L butyl ester was added, acidified with 0.2M hydrochloric acid, stirred for 5 minutes and then left to stand for 30 minutes, the water phase was removed, and the butyl ester phase was heated to cyclize, and the cyclization was stopped when the cyclization rate reached more than 97%. The butyl ester continued to be concentrated in vacuo, and when the volume was about 400ml, the temperature was lowered to crystallize at -5°C to 10°C, kept for 2 hours, and centrifuged to obtain 70g of the crude product.

[0022] The crude product was recrystallized according to the ratio of lovastatin crude product: ethanol = ...

Embodiment 2

[0024] Fermentation broth 10L, unit 6742u / ml, adjust to PH10 with 2mol / l NaOH, filter, add alkaline water continuously during the filtration process, stop filtering when the unit of the filtrate is lower than 200u / ml, collect the filtrate, and use the resin to adsorb the filtrate , desorbed with ethanol after adsorption, concentrated the desorbed solution in vacuum, added 2.5L butyl ester, acidified with 0.1M hydrochloric acid, stirred for 5 minutes and then stood still for 30 minutes, removed the water phase, and the butyl ester phase was heated and cyclized, and the cyclization rate reached 97 The cyclization is stopped when above %. The butyl ester continued to be concentrated in vacuo, and when the volume was about 350ml, the temperature was lowered to below 10°C to crystallize, kept for 2 hours, and centrifuged to obtain 62g of the crude product.

[0025] The recrystallization step is the same as that of Example 1, and 47 g of the refined product obtained has a content of...

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PUM

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Abstract

The present invention relates to extraction and purification of lovastatin by resin through the fermentation broth from cultivation of Aspergillus terreus, which comprises the following steps: (1) Alkalizing the fermentation broth to transform lovastatin into salt, thus releasing said salt from intraspore to extraspore, followed by filtering; (2) Absorbing and extracting lovastatin from the filtrate by resin; (3) Concentrating, cyclizing, and crystallizing; (4) Centrifugating, washing, and drying the crystalline sloution; (5) Recrystallizing the crude product. In the present invention, only small amount solvent is required to provide qualified lovastatin final product, moreover the whole procedure is simple and the yield is high, thus is economic and convenient to be carried out.

Description

Technical field: [0001] The invention relates to a new method for extracting and purifying lovastatin from the fermented liquid rich in lovastatin produced by cultivating Aspergillus terreus. Background technique: [0002] Patent WO9720834 describes that the fermentation broth is adjusted to alkaline with NaOH, and then extracted with a mixed solvent of toluene and ethanol under the condition of stirring. After washing the extract, add toluene and perlite, acidify with nitric acid, add chloroform after stirring, compress and filter, then add chloroform and heat to complete the cyclization. The crude product was recrystallized after concentration and crystallization. There are disadvantages in this method: too many solvents are used, and mixed solvents are used, which brings certain difficulties to solvent recovery. At the same time, it brings great pressure to the environment. The emulsification is serious during extraction, which brings certain problems to the separation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/30
Inventor 宋爱刚孙玫周雄兵秦永忠秦娜佳
Owner SHANDONG LUKANG PHARMA
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