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Preparation method of cordycepin crystal

A technology of cordycepin and crystal, applied in the field of medicinal chemistry, can solve the problems of complicated operation, low extraction rate and high production cost, and achieve the effect of simple operation and high product purity

Inactive Publication Date: 2015-02-04
NORTHWEST A & F UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Cordycepin is the main physiologically active component of Cordyceps militaris. It is a nucleoside substance composed of adenine and deoxypentose. It has great market prospects in medical care. Currently, Cordycepin is extracted from Cordyceps militaris Extracted by complex processes, including water bath, alcohol bath extraction, resin adsorption, chromatography separation, activated carbon adsorption, etc., these methods are either complex in operation, low in extraction rate, or require different resin treatments or require With the help of expensive HPLC preparative chromatography equipment, the production cost is high and it is difficult to realize large-scale industrial production
[0004] In recent years, the field has tried to obtain high-purity flaky cordycepin crystals by cultivating the residues of Cordyceps militaris, but this method has a low yield and a large waste of raw materials

Method used

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  • Preparation method of cordycepin crystal
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  • Preparation method of cordycepin crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: Prepare cordycepin crystals according to the following steps:

[0024] (1) Naturally drying and pulverizing the remaining substrate of the cultured Cordyceps militaris sporozoites, and then passing through an 80-mesh sieve for subsequent use;

[0025] (2) Weigh 20 g of Cordyceps militaris powder, add 5 times the volume of 50% ethanol solution, and extract in an alcohol bath at 60° C. for 5 hours;

[0026] (3) centrifuge 10min under the condition of 3000r / min with a high-speed centrifuge, collect the supernatant for subsequent use;

[0027] (4) Purify the supernatant collected after centrifugation with macroporous resin, sample liquid and NKAII macroporous resin are loaded with the amount of 50ml: 1g, pH 5, 1.8BV / h, then remove impurities with 5BV of distilled water, The flow rate is 1.8BV / h, and finally eluted with 5BV of 50% ethanol solution, pH 3, and the flow rate is 1.8BV / h;

[0028] (5) Use ethanol eluent and ammonium sulfate to form a two-phase sys...

Embodiment 2

[0033] Embodiment 2: Prepare cordycepin crystals according to the following steps:

[0034] (1) Naturally drying and pulverizing the remaining substrate of the cultured Cordyceps militaris sporozoites, and then passing through an 80-mesh sieve for subsequent use;

[0035] (2) Weigh 20 g of Cordyceps militaris powder, add 6 times the volume of 60% ethanol solution, and extract in an alcohol bath at 60° C. for 4 hours;

[0036] (3) Centrifuge for 15min under the condition of 3000r / min with a high-speed centrifuge, and collect the supernatant for subsequent use;

[0037] (4) purify the supernatant collected after centrifugation with macroporous resin, sample liquid and NKAII macroporous resin are loaded with the amount of 50ml: 1.2g, 1.8BV / h, then remove impurities with the distilled water of 5BV, flow velocity is 1.8BV / h, finally eluted with 5BV of 50% ethanol solution, the flow rate is 1.8BV / h;

[0038] (5) Use ethanol eluent and ammonium sulfate to form a two-phase system, w...

Embodiment 3

[0043] Embodiment 3: Prepare cordycepin crystals according to the following steps:

[0044] (1) Naturally drying and pulverizing the remaining substrate of the cultured Cordyceps militaris sporozoites, and then passing through an 80-mesh sieve for subsequent use;

[0045] (2) Weigh 20g of Cordyceps militaris powder, add 4 times the volume of 70% ethanol solution, and extract in an alcohol bath at 60°C for 6h;

[0046] (3) Centrifuge for 15min under the condition of 3000r / min with a high-speed centrifuge, and collect the supernatant for subsequent use;

[0047] (4) purify the supernatant collected after centrifugation with macroporous resin, sample liquid and NKAII macroporous resin are loaded with the amount of 50ml: 0.8g, 1.5BV / h, then remove impurities with the distilled water of 4BV, flow velocity is 1.6BV / h, finally eluted with 7BV of 40% ethanol solution, the flow rate is 2BV / h;

[0048] (5) Use ethanol eluent and ammonium sulfate to form a two-phase system, wherein the...

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Abstract

The invention discloses a preparation method of a cordycepin crystal. The preparation method includes following steps: (1) with residual substrate after cultivation of cordyceps militaris stroma as a raw material, crushing the substrate, performing extraction with an organic solvent and performing centrifugation to collect a supernate; (2) performing purification to a crude liquid after the centrifugation through a macroporous resin adsorption chromatographic column; (3) performing enrichment to the cordycepin obtained through the step (2) with an aqueous two-phase system composed of ethanol and ammonium sulfate; and (4) performing elution in a chromatographic column with a methanol solution, performing reduced pressure distillation for concentrating an eluent, performing methanol elution to the concentrated eluent, and performing crystallization to the eluent to obtain the cordycepin crystal. The preparation method of the cordycepin crystal is reduced in production cost, increases the purity of the cordycepin and is free of residual organic solvent.

Description

technical field [0001] The invention relates to a preparation method of cordycepin and its crystal, belonging to the field of medicinal chemistry. Background technique [0002] Cordyceps militaris is a model species of Ascomycetes, Ergotaceae, Ergotaceae, and Cordyceps genus. Yin, but also nourishes kidney yang, mainly treats kidney deficiency, impotence and nocturnal emission, sore waist and knees, weakness after illness, chronic cough and weakness, coughing up phlegm and blood, spontaneous sweating, etc. It is the only traditional Chinese medicine that can balance and regulate yin and yang at the same time. widely. [0003] Cordycepin is the main physiologically active component of Cordyceps militaris. It is a nucleoside substance composed of adenine and deoxypentose. It has great market prospects in medical care. Currently, Cordycepin is extracted from Cordyceps militaris Extracted by complex processes, including water bath, alcohol bath extraction, resin adsorption, ch...

Claims

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Application Information

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IPC IPC(8): C07H19/16C07H1/08
CPCY02P20/582C07H19/16C07H1/08
Inventor 秦宝福王建刚杜双田刘霞谭珍珍郑立飞王阳吴养会曹让陈晓红
Owner NORTHWEST A & F UNIV