Anthricin preparation method

A technology of ginseng lactone and acetaminophen, applied in the field of biotechnology chemistry, can solve the problems of low sample yield, complicated operation, small preparation amount and the like

Inactive Publication Date: 2013-12-04

NANJING BIAOKE BIO TECH

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AI-Extracted Technical Summary

Problems solved by technology

Due to the complicated operation, small amount of preparation and ...

Abstract

The invention discloses an anthricin preparation method. The method includes the following steps: 1), taking anthricin for smashing, adding 5-10 times of amount of 30-90% ethanol solution, performing reflux extraction for 2-3 times, concentrating an extracting solution to be alcohol-free, adding the extraction solution in macroporous resin for adsorption, using ethanol solution for gradient elution, collecting eluent, depressurizing for concentration, adding benzene solution in size volume and fully stirring, collecting a benzene solution layer to be concentrated to a small size, and placing for crystallization; 2), dissolving obtained crystals by 5-10 times of amount of 80-90% methanol, adding activated carbon for decoloring, concentrating filtrate to enable alcohol concentration to be 30-50%, extracting by benzene solution, adding 1/3-1/10 ethanol solution in extract liquor, placing for recrystallizing, and drying crystal substances to obtain anthricin. The anthricin preparation method is simple and convenient in process operation, low in production cost and easy to realize industrial production.

Application Domain

Organic chemistry

Technology Topic

Activated carbonChemistry +9

Examples

Experimental program(4)

Example Embodiment

[0013] Example 1:

[0014] Take 10kg of Eshen smashed, add 5 times the amount of 70% ethanol solution, reflux and extract 3 times, combine the extracts to shrink to no alcohol and add them to AB-8 macroporous resin for adsorption, first eluting with 8 times the column volume of 30% ethanol, and then Elute with 7 times the column volume of 75% ethanol solution, collect the eluate, concentrate under reduced pressure, add an equal volume of benzene solution to the concentrated solution and stir well, and concentrate the collected benzene solution layer to a small volume for crystallization. The obtained crystals are dissolved in 10 times the amount of 80% methanol, added with activated carbon for decolorization, the filtrate is concentrated to an alcohol concentration of 30%, and then extracted with benzene solution twice. The extract is added with 1/3 ethanol solution and left to recrystallize. The crystals are 3.5g of Eginsenolide Detected by HPLC, the content is 98.6%.

Example Embodiment

[0015] Example 2:

[0016] Take 10kg of Eshen smashed, add 10 times the amount of 30% ethanol solution, reflux and extract twice, combine the extracts to shrink to no alcohol and add them to D101 macroporous resin for adsorption, first eluting with 5 times the column volume of 20% ethanol, and then 10 Elute the column volume with 70% ethanol solution, collect the eluate, concentrate under reduced pressure, add an equal volume of benzene solution to the concentrate and stir well, and concentrate the collected benzene solution layer to a small volume for crystallization. The obtained crystals were dissolved in 5 times the amount of 90% methanol, added with activated carbon for decolorization, the filtrate was concentrated to an alcohol concentration of 50%, and then extracted with benzene solution twice. The extract was added with 1/10 ethanol solution and left to recrystallize. The crystallized product was 3.1 g of Eginsenolide Detected by HPLC, the content is 97.4%.

Example Embodiment

[0017] Example 3:

[0018] Take 10kg of Eshen smashed, add 10 times the amount of 90% ethanol solution, reflux for 2 times, combine the extracts to shrink to no alcohol, add an appropriate amount of aqueous solution, and then add to HZ816 macroporous resin for adsorption, first wash with 5 times the column volume of 50% ethanol After removing, eluting with 10 times the column volume of 75% ethanol solution, collecting the eluate, concentrating under reduced pressure, adding an equal volume of benzene solution to the concentrated solution and stirring thoroughly, collecting the benzene solution layer and concentrating to a small volume for crystallization. The obtained crystals were dissolved in 8 times the amount of 80% methanol, added with activated carbon for decolorization, the filtrate was concentrated to an alcohol concentration of 40%, and then extracted with benzene solution twice. The extract was added with 1/5 ethanol solution and allowed to recrystallize. The crystallized product was 3.9g of Eginsenolide Detected by HPLC, the content is 98.1%.

PUM

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