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Preparation method of astragaloside acid

A technology of astragaloside IV and astragaloside IV is applied in the directions of steroids, organic chemistry, etc., and can solve the problems such as difficulty in obtaining pure astragaloside IV, complicated steps, side reactions and the like

Pending Publication Date: 2020-08-18
CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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  • Abstract
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  • Claims
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Problems solved by technology

[0003] In the prior art, after preparing astragaloside IV under alkaline conditions, before preparing it into astragaloside, it is necessary to separate and purify astragaloside IV first, and then perform subsequent oxidation and other operations. Not only the steps are cumbersome, but also the existing It is also difficult to obtain astragaloside IV with high purity in the separation and purification process, and it is easy to introduce impurities into the subsequent oxidation and other processes, thereby causing side reactions

Method used

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  • Preparation method of astragaloside acid

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preparation example Construction

[0024] The invention provides a brand-new preparation method of astragaloside. Specifically include the following steps:

[0025] 1. Take the dry product of Astragalus membranaceus, crush it, and extract it three times with ethanol with a concentration of 30-95% at a solid-to-liquid ratio (g / mL) of 1:6-1:15, each time for 90 minutes.

[0026] 2. Combine the extracts, reclaim ethanol under reduced pressure, add water to dilute, and the solid-liquid ratio of water consumption to the quality of the Radix Astragali medicinal material is 0.5-2 (g / mL). After extracting twice with an equal volume of ethyl acetate, the extracted aqueous phase was passed through a D101 macroporous resin column. The quality of the resin column is the same as that of the Radix Astragali. Wash once with deionized water of 3 times the volume of the resin column, and then elute once with 70% ethanol of 3 times the volume of the resin column. The ethanol eluate was collected, and the ethanol was recovered...

Embodiment

[0032] Example: Preparation of Astragaloic Acid

[0033] 1. Take 10Kg of the dry product of Astragalus membranaceus, crush it, and extract it three times with 70% ethanol at a ratio of solid to liquid (g / mL) of 1:10, each time for 90 minutes.

[0034] 2. Combine the extracts, recover ethanol under reduced pressure, add water to dilute, the water consumption is based on the mass of Astragalus medicinal material, and the ratio of solid to liquid is 1:2 (g / mL). Pass the diluted aqueous solution through a D101 macroporous resin column, and the weight of the resin column is 10kg. Wash once with deionized water of 3 times the volume of the resin column, and then elute once with 70% ethanol of 3 times the volume of the resin column. The ethanol eluate was collected, and the ethanol was recovered under reduced pressure.

[0035] 3. Add 2 L of 50% tetrahydrofuran aqueous solution (THF) for dispersion. Subsequently, 10 g of sodium hydroxide was added, and alkaline hydrolysis was carr...

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Abstract

The invention belongs to the field of compound synthesis, and particularly relates to a preparation method of astragaloside acid. The method specifically comprises the following steps: adding or generating a pH buffer system into an astragaloside-containing reaction system obtained by performing a resin treatment on an astragalus extract and performing alkaline hydrolysis, and adding an oxidant tocarrying out oxidation to obtain the astragaloside acid. A carbonate / bicarbonate buffer system is added or generated after alkaline hydrolysis for the first time so as to ensure that the reaction isalways carried out in a required weakly alkaline environment; astragaloside is directly oxidized in a reaction system containing astragaloside. Astragaloside does not need to be extracted, separated,purified and then subjected to subsequent reactions.

Description

technical field [0001] The invention belongs to the field of compound synthesis, and in particular relates to a preparation method of astragalinic acid. Background technique [0002] There are a large number of astragaloside derivatives in Astragalus medicinal materials, and these derivatives will be hydrolyzed into astragaloside IV under alkaline conditions. Astragaloside IV is one of the main active components of Astragalus, which has various pharmacological effects such as improving cardiopulmonary function and enhancing body immunity. Astragaloside is the C on the glucose group in the astragaloside IV molecule 6 The product obtained after directional oxidation of hydroxymethyl group to carboxyl group; compared with astragaloside IV, it has better druggability. [0003] In the prior art, after preparing astragaloside IV under alkaline conditions, before preparing it into astragaloside, it is necessary to separate and purify astragaloside IV first, and then perform subse...

Claims

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Application Information

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IPC IPC(8): C07J53/00
CPCC07J53/004
Inventor 青琳森丁立生罗培彭树林梁健
Owner CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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