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A kind of extraction and refining process of mevastatin

A technology of mevastatin and extraction tank, applied in the direction of organic chemistry, etc., can solve the problems of increasing production cost, waste, increasing economic pressure, etc.

Active Publication Date: 2015-08-05
LIVZON NEW NORTH RIVER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] As can be seen from the above, the present mevastatin separation and extraction process all has the problem of low total yield of mevastatin extracted from the fermentation broth, and the lower yield of mevastatin will not only cause great waste, but also cause Invisibly increase its production cost, which is not conducive to the reduction of the price of statin drugs with mevastatin as the precursor, thus increasing the economic pressure on users of such drugs

Method used

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  • A kind of extraction and refining process of mevastatin
  • A kind of extraction and refining process of mevastatin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Experiment A

[0054] 5L of isobutyl acetate was mixed with 5L of water, and added continuously to the mevastatin-containing fermentation broth (10L) after 0.5h. Adjust pH 9.0-9.6 with concentrated NaOH. The mixture was heated to 60°C and maintained at this temperature for 2 hours. The organic and aqueous phases were separated by countercurrent separation. Sodium lauryl sulfate was added to help emulsify the mixture upon separation.

[0055] The pH of the purified fermentation broth was adjusted to 2.0-4.5 with sulfuric acid. 5L of isobutyl acetate was continuously added to the fermentation broth, and the isobutyl acetate phase containing mevastatin was continuously separated.

[0056] The isobutyl acetate phase was concentrated to about 150 mL under vacuum. Dilute the concentrate to 800mL with NaHCO 3 washing. After washing, the concentrate was concentrated again to 150 mL. The concentrate is cooled to 0-5°C. Get mevastatin after overnight. The crude product ...

Embodiment 2

[0079] Phosphoric acid was used to adjust the pH value of 10L of fermented liquid, and the fungus residue obtained by filtering was blown dry until the water content of the fungus residue was 32%, and the filtrate was tested and then processed. Put the dried slag and toluene into the extraction tank, the ratio of toluene to slag is 6:1 (V / W), cyclization, the cyclization takes 8.5 hours, filter, wash the filter residue 3 times with toluene , and the washings were mixed with the filtrate and allowed to stand to complete the extraction. Dry the waste residue, and carry out environmental protection treatment of the waste residue and the extracted waste liquid.

[0080] The extract filtrate was distilled under reduced pressure to recover toluene and water. After the reduced-pressure distillation was completed, the temperature of the concentrated solution was lowered to 15° C., and n-hexane at the same temperature was added, kept stirring and crystallized. Filtrate, vacuumize the ...

Embodiment 3

[0085] Phosphoric acid was used to adjust the pH value to 3.7 in 10L of fermented liquid, and the fungus residue obtained by filtration was blown dry until the water content of the fungus residue was 40%, and the filtrate was tested and then processed. Put the dried bacteria residue and toluene into the extraction tank, the ratio of toluene to bacteria residue is 6:1 (V / W), cyclization, the time spent for cyclization is 7-9 hours, filter, wash the filter residue with toluene 3 times, and the washings were mixed with the filtrate and allowed to stand to complete the extraction. Dry the waste residue, and carry out environmental protection treatment of the waste residue and the extracted waste liquid.

[0086] The extract filtrate was distilled under reduced pressure to recover toluene and water. After the reduced-pressure distillation was completed, the temperature of the concentrated solution was lowered to 15°C, and organic solvent A at the same temperature was added, kept st...

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Abstract

The invention provides a method for extracting and refining Mevastatin from fermentation liquid. The method is characterized by comprising the following steps of: pretreating the fermentation liquid containing the Mevastatin by using acid; and blow drying fungus dregs. By the method, the production period is shortened, the cost is reduced, and simultaneously, the total yield of the Mevastatin is improved.

Description

technical field [0001] The invention relates to a method for isolating or purifying mevastatin or a pharmaceutically acceptable salt thereof from microbial fermentation liquid. Background technique [0002] Mevastatin (mevastatin, as shown in formula 1), also known as compactin (compactin), ML-236B, is a 3-hydroxy 3-methylglutaryl coenzyme A reductase (HMG-CoA) inhibitor, It was accidentally extracted from the culture medium of fungi (Penicillium Citrinum) by Biochemist Endo of Sankyo Pharmaceutical Company in Japan, and its chemical name is 2-methylbutyric acid-{1S-[1α(R), 7β, 8β(2S, 4S ), 8aβ]}-1,2,3,7,8,8a-hexahydro-7-methyl-8{2-[4-hydroxy-6-oxo-2H-tetrahydropyranyl]-B Base}-1-naphthyl ester, the specific structural formula is as follows: [0003] [0004] Mevastatin is the first generation of statins, and now it is mostly used as the precursor of pravastatin, an active statin drug. Therefore, the yield and quality of mevastatin directly affect the cost and purity of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/30
Inventor 唐阳刚李敬辉张起智卢创向双
Owner LIVZON NEW NORTH RIVER PHARMA