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Method for preparing high-purity danshinolic acid B

A salvianolic acid, high-purity technology, applied in the field of extracting high-purity salvianolic acid B, can solve the problems of not too high salvianolic acid B purity, cumbersome operation process, complicated process, etc.

Inactive Publication Date: 2010-02-03
SHANGHAI INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The main disadvantage of macroporous adsorption resin separation is the low purity of the prepared salvianolic acid B sample
CN1247855A discloses the preparation method of salvianolic acid magnesium salt, its main active ingredient is salvianolic acid B magnesium salt, but its content can only reach 60%
The extraction process of salvianolic acid B disclosed in CN1240695C uses silica gel column chromatography to separate and purify salvianolic acid B to obtain salvianolic acid B with a purity of 50%-96%, but the process is complicated and the cost of silica gel column chromatography is relatively high , the operation process is cumbersome, and it is difficult to expand to production
But its process is complex and costly
In CN1876641A, the salvia miltiorrhiza was treated with microwaves, centrifuged to remove the precipitate, then applied to polyamide resin, and ethanol gradient elution was used to obtain salvianolic acid B with a purity of 95%. The purity of the salvianolic acid B was not too high, and there was no mention its yield

Method used

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  • Method for preparing high-purity danshinolic acid B
  • Method for preparing high-purity danshinolic acid B
  • Method for preparing high-purity danshinolic acid B

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preparation example Construction

[0045] The preparation method of the high-purity salvianolic acid B provided by the invention comprises steps:

[0046] (1) the water extract of Salvia miltiorrhiza 20-70g and 10 9 -10 10 Individuals / ml of Fusarium graminearum (Fusarium graminearum) resting cells were contacted and placed at 20-35°C for 24-90 hours to obtain an aqueous extract of Salvia miltiorrhiza from which rosmarinic acid was removed; and

[0047] (2) The water extract of Salvia miltiorrhiza from which rosmarinic acid was removed was adsorbed by reversed-phase resin and eluted with water or methanol aqueous solution to obtain high-purity salvianolic acid B.

[0048] Preferably, 40-50g of salvia miltiorrhiza water extract and 5×10 9 -10 10 pcs / ml 10 9 Resting cells are mixed.

[0049] Preferably, air is introduced at 22-32°C, stirred or oscillated for 30-80 hours to obtain the aqueous extract of Danshen from which rosmarinic acid has been removed; more preferably, air is introduced at 25-30°C, stirred ...

Embodiment 1

[0080] Weigh 100g of dried salvia miltiorrhiza (salvianolic acid B content 2%), add 400ml of water to extract twice at 90°C, combine the two filtrates, concentrate under reduced pressure to 50ml, adjust pH2, add 50ml ethyl acetate to extract twice, combine the two filtrates Ethyl acetate solution was concentrated to recover ethyl acetate. Dissolve the concentrated residue in 200ml of pH7 phosphate buffer, add 10g of wet cells of Fusarium graminearum, shake on a shaker at 28°C, transform for 36 hours, and obtain a crude extract of salvianolic acid without rosmarinic acid . The crude extract was sterilized by filtration, adjusted to pH 2, allowed to stand still to precipitate impurities, filtered and then applied to reversed-phase resin XAD-2, with a resin volume of 200ml. After the column is applied, 1000ml of water is used to elute the resin column, and then 45% methanol is used to elute the resin column until the impurities whose retention time is less than salvianolic acid ...

Embodiment 2

[0087]Weigh 100g of dried salvia miltiorrhiza (salvianolic acid B content 2%), add 400ml of water to extract twice at 90°C, combine the two filtrates, concentrate under reduced pressure to 50ml, adjust pH2, add 50ml ethyl acetate to extract twice, combine the two filtrates Ethyl acetate solution was concentrated to recover ethyl acetate. Dissolve the concentrated residue in 200ml of pH7 phosphate buffer, add 10g of wet cells of Fusarium graminearum, shake on a shaker at 28°C, transform for 36 hours, and obtain a crude extract of salvianolic acid without rosmarinic acid . Filter and sterilize the crude extract, then adjust the pH to 2, let stand to precipitate impurities, adjust the filtrate to pH 7 after filtration, apply reverse phase resin HP-20, and wash with water to collect salvianolic acid B eluate with a purity of 99%. , combined, adjusted to pH 2, extracted with ethyl acetate to remove salt, recovered ethyl acetate, dissolved salvianolic acid B in water, and lyophiliz...

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Abstract

The invention discloses a method for preparing high-purity danshinolic acid B, which comprises the following steps: (1) mixing a red sage root aqueous extract with Fusarium graminearum resting cells,and performing biotransformation at a temperature of between 20 and 35 DEG C for 24 to 90 hours to obtain a red sage root aqueous extract without rosmarinic acid; and (2) adsorbing the red sage root aqueous extract without the rosmarinic acid by anti-phase resin, and eluting the red sage root aqueous extract without the rosmarinic acid to obtain the high-purity danshinolic acid B. The purity of the danshinolic acid B prepared by the method is more than or equal to 99 percent, the recovery percent is over60 percent, the process is simple, and the cost is low.

Description

technical field [0001] The invention relates to the field of plant purification, in particular to a method for extracting high-purity salvianolic acid B from salvia miltiorrhiza. Background technique [0002] The existing separation and purification methods of salvianolic acid B are mainly separated by macroporous adsorption resin or high-speed countercurrent chromatography. [0003] The main disadvantage of macroporous adsorption resin separation is the low purity of the prepared salvianolic acid B sample. CN1247855A discloses a preparation method of salvianolic acid magnesium salt, the main active ingredient of which is salvianolic acid B magnesium salt, but its content can only reach 60%. The extraction process of salvianolic acid B disclosed in CN1240695C uses silica gel column chromatography to separate and purify salvianolic acid B to obtain salvianolic acid B with a purity of 50%-96%, but the process is complicated and the cost of silica gel column chromatography is ...

Claims

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Application Information

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IPC IPC(8): C07D307/84C12P17/04C12R1/01
Inventor 李继安阚士东陈代杰
Owner SHANGHAI INST OF PHARMA IND
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