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Preparation method of 1, 4-succinic acid adenosine methionine

A technology of adenosylmethionine succinate and adenosylmethionine, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problem of inability to ensure that the product meets the relevant raw material drug standards, unstable product quality, Complicated preparation methods and other issues, to achieve the effects of high product yield, white color, and simple operation

Active Publication Date: 2015-03-18
SHANGHAI INST OF PHARMA IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem solved by the present invention is to overcome the complex preparation method of 1,4-butanedisulfonic acid adenosylmethionine in the prior art, the unstable product quality, low purity, and the inability to guarantee that the prepared product meets the relevant raw material drug standards, etc. Deficiency, provide a kind of preparation method of 1,4-butanedisulfonic acid adenosylmethionine

Method used

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  • Preparation method of 1, 4-succinic acid adenosine methionine

Examples

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Embodiment 1

[0045] A preparation method of 1,4-butanedisulfonic acid adenosylmethionine, which comprises the steps of:

[0046] (1) Fermentation and cultivation of adenosylmethionine-producing bacteria, the specific steps are as follows:

[0047] 1) Saccharomyces cerevisiae CPCC340488 was inoculated on the slant medium for slant culture, cultured at 30°C for 3 days, and then refrigerated at 4°C for 5 days to obtain a well-grown slant; the slant medium contained: soybean peptone 2.0wt% , yeast extract 0.5wt%, glucose 2.0wt% and agar strip 2.0wt%, the pH value of the slant medium is 6.0;

[0048] 2) Add 20mL of sterile water to the growing slope, scrape it off with a sterile inoculation stick, place it in a shaker and vibrate evenly, then insert the seed medium with an inoculation amount of 0.5mL / 250mL bottle, and carry out seed cultivation. Cultivate on a shaking table at 250 rpm for 24 hours at 28°C; wherein, the seed medium contains: 2.0wt% glucose, 1.0wt% yeast extract and 2.0wt% soybe...

Embodiment 2

[0058] A preparation method of 1,4-butanedisulfonic acid adenosylmethionine, which comprises the steps of:

[0059] (1) Fermentation and cultivation of adenosylmethionine-producing bacteria, the specific steps are as follows:

[0060] 1) Saccharomyces cerevisiae CPCC340488 was inoculated on the slant medium for slant culture, cultured at 30°C for 3 days, and then refrigerated at 4°C for 5 days to obtain a well-grown slant; the slant medium contained: soybean peptone 2.0wt% , yeast extract 0.5wt%, glucose 2.0wt% and agar strip 2.0wt%, the pH value of the slant medium is 6.0;

[0061] 2) Add 20mL sterile water to the well-grown slope, scrape it off with a sterile inoculation stick, place it in a shaker and oscillate evenly, then insert the inoculation amount of 1.5mL / 750mL bottle into the seed medium, and carry out seed cultivation. Cultivate on a shaking table at 250 rpm for 24 hours at 28°C; wherein, the seed medium contains: 2.0wt% glucose, 1.0wt% yeast extract and 2.0wt% so...

Embodiment 3

[0071] A preparation method of 1,4-butanedisulfonic acid adenosylmethionine, which comprises the steps of:

[0072] (1) Fermenting and culturing the adenosylmethionine-producing bacteria, the specific operation steps are the same as in Example 2;

[0073] Use oxalic acid to adjust the pH value of the fermented liquid to 3.0, and obtain 15L of wet cells after plate and frame filtration. After the wet cells are dried by cold wind until the water content is 10wt%, freeze-thaw treatment is carried out twice. The method of freeze-thaw treatment is as follows: Freeze the wet cells at -80°C for 24 hours, then thaw at 20-25°C for 4 hours; mix 75L of sulfuric acid aqueous solution with a pH value of 4 and the wet cells after freezing and thawing, and place them at 0-10°C for 3 hours. Obtain the acid solution containing the wall-broken bacteria;

[0074] (2) At 0-10°C, filter the acid solution containing broken-wall bacteria in a ceramic membrane, and add an aqueous solution of oxalic ...

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Abstract

The invention discloses a preparation method of 1, 4-succinic acid adenosine methionine. The preparation method comprises the following steps: acidifying and filtering a fermentation solution of adenosyl methionine-producing bacteria to obtain wet thalli, drying, performing freezing and thawing treatment, and uniformly mixing a water solution of inorganic strong acid with the wet thalli; filtering an acid solution containing wall-broken thalli in a ceramic membrane, adding the water solution of inorganic strong acid, and collecting filtrate; filtering the filtrate by a nano-filtration membrane to obtain a concentrated solution A; passing through a medium polar macroporous adsorption resin column, and washing with water, thereby obtaining effluent B; passing through an H+ type macroporous weakly acidic cation exchange resin column, performing elution on the H+ type macroporous acidic cation exchange resin column with 1, 4-succinic acid, performing distributed collection, and merging effluent C; sequentially filtering a collected solution by an ultra-filtration membrane and the nano-filtration membrane; and mixing a concentrated solution D with 1, 4-succinic acid, regulating the proportion of 1, 4-succinic acid to adenosyl methionine, and drying to obtain 1, 4-succinic acid adenosine methionine. The preparation method disclosed by the invention has the advantages of simplicity in operation, relatively high product yield, white color and luster and high purity.

Description

technical field [0001] The invention relates to a preparation method of 1,4-butanedisulfonic acid adenosylmethionine. Background technique [0002] 1,4-butanedisulfonine (S-adenosyl-L-methionnine1,4-butanedisulfonate) is the 1,4-butane of S-adenosyl-L-methionine (SAM, SAMe) Disulfonate is clinically used to treat depression, arthritis, liver dysfunction and other diseases. It is suitable for intrahepatic cholestasis before cirrhosis and cirrhosis; it is suitable for intrahepatic cholestasis during pregnancy. [0003] Its chemical name: (±)-5'-[(R*)-[(R*)-3-amino-3-carboxypropyl]methylsulfonyl]-5'-deoxyadenosine 1,4-butane Disulfonate. Its molecular formula is: C 15 h 23 N 6 o 5 S + ·C 4 h 9 o 6 S 2 0.65C 4 h 10 o 6 S 2 ; Its molecular weight is 748.24. For the specific structural formula, please refer to the Chinese patent application CN201210126839.0. [0004] Chinese patent CN200510019206.x, US patents USP4990606, USP5128249 and European patent EP0162323 a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/167C07H1/00C07H1/08
CPCC07H1/00C07H1/08C07H19/167
Inventor 李继安陈代杰陈舟舟林惠敏胡敏赵运霞张琼李亚军
Owner SHANGHAI INST OF PHARMA IND CO LTD
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