A kind of extraction method of mycophenolic acid

An extraction method, the technology of mycophenolic acid, applied in the direction of organic chemistry, etc., can solve the problems of increasing production cost, increasing production difficulty, and large loss of mycophenolic acid, and achieves the effect of not being easy to recycle, reducing refining steps, and simple method

Active Publication Date: 2016-03-23
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are following disadvantages in the above-mentioned technology: for example, the loss of extracting mycophenolic acid with ethanol is relatively large, so that more mycophenolic acid remains in the waste residue, so the yield is low, and by-products are easily produced; ethanol and ethyl acetate are volatile Strong, low boiling point, dangerous, not easy to recycle, thus increasing production difficulty and increasing production cost

Method used

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  • A kind of extraction method of mycophenolic acid

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Effect test

Embodiment 1

[0070] 10L of mycophenolic acid fermentation broth (fermentation unit: 4978μg / ml) was adjusted to pH 10 with 15% (w / v) NaOH, and filtered. Turn on the stirring, add CaCl of 1% (w / v) of the filtrate volume to the filtrate 2 , adjust the pH to 3.0 with 5mol / L HCl solution, let it settle for 30 minutes, add 20g of perlite filter aid, stir evenly, and filter to obtain a filter cake.

[0071] Dry the filter cake at 40°C, crush the dried 1000g filter cake, put it into the extraction barrel, add 3L butyl acetate, stir and extract at 45°C for about 1 hour, and then use the suction filter to dry the material , to obtain the filtrate. The extraction was repeated 2 more times under the above conditions. Afterwards, the obtained filtrate was concentrated by a thin-film concentrator, the material temperature was 65° C., and the vacuum degree was -0.08 Mpa to obtain 3.1 L of concentrated liquid. Add activated carbon with 2% (w / v) volume of the concentrated solution, and decolorize at 40°...

Embodiment 2

[0075] 10L of mycophenolic acid fermentation broth (fermentation unit: 4898μg / ml) was adjusted to pH 11 with 15% (w / v) NaOH, and filtered. Turn on the stirring, add CaCl of 2% (w / v) of the filtrate volume to the filtrate 2 , adjust the pH to 3.2 with 5mol / L HCl solution, let it settle for 40 minutes, add 20g of perlite filter aid, stir evenly, and filter to obtain a filter cake.

[0076] Dry the filter cake at 42°C, crush the dried 1000g filter cake, put it into the extraction barrel, add 3L butyl acetate, stir and extract at 48°C for 1.5 hours, and then use the suction filter to dry the material. A filtrate was obtained. The extraction was repeated 2 more times under the above conditions. Afterwards, the obtained filtrate was concentrated using a thin-film concentrator, the material temperature was 70° C., and the vacuum degree was -0.08 Mpa to obtain 3.0 L of concentrated liquid. Add activated carbon with 4% volume of the concentrated solution, and decolorize at 45°C for ...

Embodiment 3

[0080]10L of mycophenolic acid fermentation broth (fermentation unit: 7050 μg / mL) was adjusted to pH 12 with 16% (w / v) NaOH, and filtered. Turn on the stirring, add CaCl of 2% (w / v) of the filtrate volume to the filtrate 2 , adjust the pH to 3.5 with 5mol / l HCl solution, let it settle for 50 minutes, add 20g of perlite filter aid, stir evenly, and filter to obtain a filter cake.

[0081] Dry the filter cake at 45°C, crush the dried 1000g filter cake, put it into the extraction barrel, add 3L butyl acetate, stir and extract at 50°C for 2 hours, and then use the suction filter to dry the material. A filtrate was obtained. The extraction was repeated 2 more times under the above conditions. Afterwards, the obtained filtrate was concentrated using a thin film concentrator, the material temperature was 75° C., and the vacuum degree was -0.08 Mpa to obtain 3.5 L of concentrated liquid. Add activated carbon with 5% (w / v) volume of the concentrated solution, and decolorize at 45°C ...

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Abstract

The invention discloses an extracting method of mycophenolic acid. The method comprises the following steps: (1), providing mycophenolic acid fermentation liquor; (2), regulating pH of the mycophenolic acid fermentation liquor to 10-12, and filtering; (3), mixing the filtrate obtained in the step (2) with calcium chloride, regulating the pH to 3.0-3.5, and filtering to obtain insoluble substances; (4), dissolving the insoluble substances in an organic solvent, and filtering to obtain filtrate; and (5), crystallizing the filtrate obtained in the step (4) to obtain a mycophenolic acid crude product. The method disclosed by the invention effectively improves yield and purity of the mycophenolic acid, and is simple, low in operation cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a method for extracting mycophenolic acid. Background technique [0002] Mycophenolic acid (also known as mycophenolic acid, English name MPA) is the precursor of mycophenolate mofetil, and its chemical name is E-4-methyl-6-(1,3-dihydro-7- Methyl-4-hydroxy-6-methoxy-3-oxo-5-isobenzofuryl)-4-hexenoic acid, the molecular formula is C 17 h 20 o 6 , the molecular weight is 320.34, the CAS number is 24280-93-1, and its structural formula is: [0003] [0004] Mycophenolic acid can efficiently, selectively, non-competitively and reversibly inhibit hypoxanthine mononucleotide dehydrogenase (IMPDH) in vivo, thereby blocking the initial synthesis pathway of guanine nucleotides and making guanine Nucleotide depletion blocks DNA synthesis. MPA selectively acts on T and B lymphocytes and inhibits their proliferation. It has been confirmed in animal kidney transplantation experime...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/88
CPCC07D307/88
Inventor 罗敏徐红张洪兰
Owner NEW FOUNDER HLDG DEV LLC
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