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Method for preparing adenosine, cordycepin and N6-(2-hydroxyethyl)adenosine simultaneously used as chemical reference substances

A technology of adenosine chemistry and cordycepin, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of cumbersome process and unreported preparation process, and achieves the effect of simple process and cost reduction.

Inactive Publication Date: 2011-05-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

Both processes are relatively cumbersome (Chinese Journal of Traditional Chinese Medicine, 2008, 33(24): 2914-2917)
However, the preparation process for obtaining three reference substances of adenosine, cordycepin, and N6-(2-hydroxyethyl)adenosine simultaneously has not been reported.

Method used

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  • Method for preparing adenosine, cordycepin and N6-(2-hydroxyethyl)adenosine simultaneously used as chemical reference substances
  • Method for preparing adenosine, cordycepin and N6-(2-hydroxyethyl)adenosine simultaneously used as chemical reference substances
  • Method for preparing adenosine, cordycepin and N6-(2-hydroxyethyl)adenosine simultaneously used as chemical reference substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Resin column separation and impurity removal

[0029] 10g of Cordyceps militaris mycelium, extracted three times with 100ml of water, the three extraction times were 1.5 hours, 1 hour, 0.5 hours respectively, combined the three extracts, recovered to about 150ml under reduced pressure, filtered through four layers of gauze, and HPD100 resin was applied to the clear liquid Column separation, wherein medicinal material: resin is 1:10 (g / ml), eluted with 3 times column volume of water, 10%, 15% ethanol solution respectively, collects 15% ethanol eluate, concentrates and dries to obtain red dip paste.

[0030] 2) Preparative HPLC purification

[0031] The red extract was dissolved in 15% methanol aqueous solution by volume fraction, configured into a 150 mg / ml test solution, and filtered through a 0.45 μm microporous membrane; the brand of preparative high-efficiency liquid phase column packing was Chromatorex C18 bonded phase packing; The diameter is 10 μm, the column...

Embodiment 2

[0033] 1) Resin column separation and impurity removal

[0034] 50g of Cordyceps militaris mycelium, extracted three times with 500ml 20% ethanol solution, the three times of extraction time were 1.5 hours, 1 hour, 0.5 hours respectively, combined three extractions, recovered to about 300ml under reduced pressure, filtered through four layers of gauze, clear liquid Separation on a Diaion resin column, wherein medicinal material: resin is 1:6 (g / ml), eluted with water, 10%, and 20% ethanol solution of 3 times the column volume respectively, and the 20% ethanol eluate is collected, concentrated and dried Get red extract.

[0035] 2) Preparative HPLC purification

[0036] The red extract is dissolved with a volume fraction of 10% methanol aqueous solution, configured into a 100 mg / ml test solution, and filtered through a 0.45 μm microporous membrane; the brand of preparative high-efficiency liquid phase column packing is Mcirosorb C18 bonded phase packing, particle size The col...

Embodiment 3

[0038] 1) Resin column separation and impurity removal

[0039] 500g of Cordyceps militaris mycelia, extracted three times with 5000ml 40% ethanol solution, the three extraction times were 1.5 hours, 1 hour, 0.5 hours respectively, combined the three extracts, recovered under reduced pressure to about 3000ml, filtered through four layers of gauze, clear liquid Separation on a D101 resin column, wherein medicinal material: resin is 1:6 (g / ml), eluted with 3 times column volume of water, 10%, and 25% ethanol solution respectively, and the 25% ethanol eluate is collected, concentrated and dried Get red extract.

[0040] 2) Preparative HPLC purification

[0041]The red extract is dissolved in 20% methanol aqueous solution by volume fraction, configured into a 50 mg / ml test solution, and filtered through a 0.45 μm microporous membrane; the brand of preparative high-performance liquid phase column packing is Chromatorex C18 bonded phase packing; particle size 10μm, column length 2...

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Abstract

The invention relates to a new preparation technology for preparing adenosine, cordycepin and N6-(2-hydroxyethyl)adenosine chemical reference substances simultaneously which are three chemical reference substances. The preparation technology is that the two-step efficient purification of Cordyceps militaris extract is performed to obtain the three chemical reference substances of which purities are more than 98%, wherein the two-step efficient purification contains resin column separation and high performance liquid chromatography. The preparation technology has simple process steps and high purity and is easy to perform large-scale production.

Description

[0001] Technical field The present invention relates to a new method for simultaneously preparing adenosine, cordycepin, and N6-(2-hydroxyethyl)adenosine chemical reference substances. It mainly includes column separation, concentration and enrichment, and rapid high-efficiency liquid phase preparation method purification. The structural formulas of the three reference substances are as follows: [0002] Background technique [0003] Cordyceps militaris is a substitute for the precious Chinese medicine Cordyceps sinensis. The two have similar ingredients and effects, and both have the effects of nourishing the kidneys and lungs, stopping bleeding and reducing phlegm. The contained nucleoside components are its main active components and quality control index components. Therefore, the preparation of high-purity nucleoside compounds is of great significance for in-depth study of their pharmacological effects and quality control of related Cordyceps medicinal materials. [0...

Claims

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Application Information

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IPC IPC(8): C07H19/16C07H1/08
Inventor 肖红斌王莉彭杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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