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Method for large-scale preparation of adenosine chemical reference substance from fruiting bodies of Armillaria chrysogenum

A yellow-green honey fungus seed, adenosine chemistry technology is applied in the field of preparation of adenosine chemical reference substances, can solve the problems of large recrystallization loss, no literature report, low recovery rate, etc., and achieves easy operation and low price. , The effect of easy batch preparation

Inactive Publication Date: 2017-10-10
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the number of silica gel column chromatography is at least 3 to 5 times, the process is cumbersome and the recrystallization loss is relatively large (the recovery rate is low), and the research on the preparation of adenosine by large-scale purification has not been reported in the literature

Method used

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  • Method for large-scale preparation of adenosine chemical reference substance from fruiting bodies of Armillaria chrysogenum
  • Method for large-scale preparation of adenosine chemical reference substance from fruiting bodies of Armillaria chrysogenum
  • Method for large-scale preparation of adenosine chemical reference substance from fruiting bodies of Armillaria chrysogenum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 The method for large-scale preparation of adenosine chemical reference substance from Armillaria chrysanthemum fruiting body comprises the following steps:

[0025] ⑴ Alcohol precipitation and impurity removal:

[0026] After dissolving 100 g of the water extract of Armillaria chrysanthemum fruiting body (brown black solid) with 5 times its mass in water, alcohol precipitation was carried out with an ethanol solution with a volume fraction of 60%, and the filtrate A was obtained by filtration, and the filtrate A was subjected to vacuum 0.06 MPa, the temperature is 70 ℃ and dried under reduced pressure to obtain 25.20 g of brown-yellow extract.

[0027] ⑵ Microporous resin (MCI) column enrichment:

[0028] The brownish yellow extractant was dissolved in ethanol solution with a volume fraction of 5 times its mass, and filtered through filter paper to obtain filtrate B; after the filtrate B was separated on a microporous resin (MCI) column, it was washed with 5 ...

Embodiment 2

[0034] Example 2 The method for large-scale preparation of adenosine chemical reference substance from Armillaria chrysanthemum fruiting body comprises the following steps:

[0035] ⑴ Alcohol precipitation and impurity removal:

[0036] After dissolving 10 g of Armillaria chrysanthemum fruiting body water extract (brown black solid) with water 10 times its mass, alcohol precipitation was carried out with ethanol solution with a volume fraction of 95%, and filtrate A was obtained by filtration, and the filtrate A was subjected to vacuum 0.09 MPa, the temperature is 50 ℃ and dried under reduced pressure to obtain 1.82 g of brown-yellow extract.

[0037] ⑵ Microporous resin (MCI) column enrichment:

[0038] The brownish-yellow extract was dissolved with 5% ethanol solution with a volume fraction 10 times of its mass, and filtered through filter paper to obtain filtrate B; after the filtrate B was separated on a microporous resin (MCI) column, it was successively washed with 2 ti...

Embodiment 3

[0044] Example 3 The method for large-scale preparation of adenosine chemical reference substance from the fruiting body of Armillaria chrysogenum, comprising the following steps:

[0045] ⑴ Alcohol precipitation and impurity removal:

[0046] After dissolving 200 g of Armillaria chrysanthemum fruiting body water extract (brown black solid) with 7 times its mass in water, alcohol precipitation was carried out with an ethanol solution with a volume fraction of 75%, and filtrate A was obtained by filtration. The filtrate A was subjected to vacuum 0.07MPa, temperature is 60 ℃ and dried under reduced pressure to obtain 48.52 g of brown-yellow extract.

[0047]⑵ Microporous resin (MCI) column enrichment:

[0048] The brown-yellow extract was dissolved with 10% ethanol solution with a volume fraction of 7 times its mass, filtered through filter paper to obtain filtrate B; after the filtrate B was separated on a microporous resin (MCI) column, it was washed with 3 times the column v...

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Abstract

The present invention relates to a method for large-scale preparation of adenosine chemical reference substance from Armillaria chrysanthemum fruiting bodies, the method comprising the following steps: (1) Alcohol precipitation and impurity removal: the aqueous extract of Armillaria chrysanthemum fruiting bodies is dissolved in water, then alcoholic precipitation, After filtering and drying under reduced pressure, a brownish-yellow extract is obtained; (2) microporous resin column enrichment: the brownish-yellow extract is dissolved in ethanol solution, filtered, and separated on a microporous resin column, followed by step gradient elution with water and ethanol solution , collect 50% ethanol water eluate, and dry the eluate under reduced pressure to obtain crude adenosine; (3) Reverse-phase liquid phase preparation chromatography purification: the crude adenosine is dissolved in methanol solution, filtered, and prepared by high-efficiency reverse-phase liquid phase The chromatographic column is separated, and the main chromatographic peak fraction in the preparation chromatogram is collected. The chromatographic peak fraction can be dried under reduced pressure to obtain the white powder adenosine reference substance. The process of the invention is simple and easy to scale.

Description

technical field [0001] The invention relates to a preparation method of an adenosine chemical reference substance, in particular to a method for large-scale preparation of an adenosine chemical reference substance from Armillaria viridans fruiting bodies. Background technique [0002] Armillaria chrysanthemum ( Armillaria luteo -rivens), commonly known as yellow mushroom, is a large wild plateau fungus, which has the functions of anti-influenza, prevention and treatment of neuritis, beriberi, promotion of children's development, anti-oxidation and anti-tumor, etc. The nucleosides and sterols contained in it are its main activities Element. So far, there is no quality control index component for Armillaria chrysanthemum. Adenosine is a nucleoside compound with a relatively high content in the fruiting body of Armillaria chrysanthemum. Due to the high polarity of this compound, it is difficult to obtain a high-purity adenosine reference substance from the fruiting body. In ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/167C07H1/06
Inventor 党军张莉王启兰梅丽娟邵赟陶燕铎岳会兰于瑞涛
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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