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Method for extracting and purifying cordycepin from cordyceps millitaris mycoderma

A technology of Cordyceps militaris and cordycepin, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of cumbersome steps, complicated experimental process, and high cost, and achieve good separation effect, simple operation, and low cost Effect

Active Publication Date: 2015-09-23
浙江中科宏寿医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The method for purifying cordycepin from the Cordyceps militaris fungus skin, the existing method is to utilize macroporous strong acid ion exchange resin to purify cordycepin, but macroporous strong acid ion exchange resin needs to be soaked several times with acid and alkali repeatedly when using, The steps are cumbersome and complicated, the amount of solvent used is large, the residue is large, and the cost of large-scale extraction is relatively high
Another method utilizes silica gel column chromatography to separate and purify cordycepin from the fruiting body of Cordyceps militaris, but its solvent is generally three-phase or four-phase, such as the combination of ethyl acetate, ethanol and water or water, ethyl acetate, isopropanol and The combination of chloroform, because there are many kinds of solvents, makes the experimental process complicated and difficult to control, and the volume ratio of the three-phase or four-phase solvents cannot be adjusted according to the density, and the solvents cannot be recycled and reused, resulting in a large amount of waste of solvents, which greatly increases cost of experiments

Method used

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  • Method for extracting and purifying cordycepin from cordyceps millitaris mycoderma
  • Method for extracting and purifying cordycepin from cordyceps millitaris mycoderma
  • Method for extracting and purifying cordycepin from cordyceps millitaris mycoderma

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1 A method of extracting and purifying cordycepin from Cordyceps militaris bacterial skin

[0043] (1), the steps are as follows:

[0044] (1) Use the Cordyceps militaris fungus skin as raw material, pulverize it with a pulverizer, pass through a 60-mesh sieve, place it in a vacuum drying oven at 40°C for 4 hours, take 1 kg, and set aside;

[0045] (2) Add 10 times the amount of 70% methanol solution to the dried Cordyceps militaris powder, and soak for 12 hours;

[0046] (3) Place the soaked suspension in a reflux device, heat and reflux 3 times, and reflux for 3 hours for the first time. After filtering with gauze, add the remaining residue to the extraction solvent, and continue heating and reflux for 2 times, 1 hour each time, Combine the filtrates to obtain the extract;

[0047] (4) The extract was extracted twice with 2 times the amount of petroleum ether, and the petroleum ether layer was discarded;

[0048] (5) the lower layer residual liquid is re...

Embodiment 2

[0064] Embodiment 2 A method of extracting and purifying cordycepin from Cordyceps militaris bacterial skin

[0065] (1), the steps are as follows:

[0066] (1) Use the Cordyceps militaris fungus skin as raw material, pulverize it with a pulverizer, pass through a 60-mesh sieve, place it in a vacuum drying oven at 40°C for 4 hours, take 1 kg, and set aside;

[0067] (2) Add 10 times the amount of 70% methanol solution to the dried Cordyceps militaris powder, and soak for 12 hours;

[0068] (3) Place the soaked suspension in a reflux device, heat and reflux 3 times, and reflux for 3 hours for the first time. After filtering with gauze, add the remaining residue to the extraction solvent, and continue heating and reflux for 2 times, 1 hour each time, Combine the filtrates to obtain the extract;

[0069] (4) The extract was extracted twice with 2 times the amount of petroleum ether, and the petroleum ether layer was discarded;

[0070] (5) the lower layer residual liquid is re...

Embodiment 3

[0075] Embodiment 3 A method of extracting and purifying cordycepin from Cordyceps militaris bacterial skin

[0076] (1), the steps are as follows:

[0077] (1) Use the Cordyceps militaris fungus skin as raw material, pulverize it with a pulverizer, pass through a 60-mesh sieve, place it in a vacuum drying oven at 40°C for 4 hours, take 1 kg, and set aside;

[0078] (2) Add 10 times the amount of 70% methanol solution to the dried Cordyceps militaris powder, and soak for 12 hours;

[0079] (3) Place the soaked suspension in a reflux device, heat and reflux 3 times, and reflux for 3 hours for the first time. After filtering with gauze, add the remaining residue to the extraction solvent, and continue heating and reflux for 2 times, 1 hour each time, Combine the filtrates to obtain the extract;

[0080] (4) The extract was extracted twice with 2 times the amount of petroleum ether, and the petroleum ether layer was discarded;

[0081] (5) the lower layer residual liquid is re...

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Abstract

The invention provides a method for extracting and purifying cordycepin from cordyceps millitaris mycoderma. The method comprises the steps that the cordyceps millitaris mycoderma is taken as raw materials and smashed through a smashing machine, screened and put in a vacuum drying box to be dried for standby use; a mixed solution of methyl alcohol and water is added in the dried cordyceps millitaris mycoderma powder for steeping; steeped suspension is arranged in a backflow device, backflow is heated and filtered, and an extraction solution is obtained; the extraction solution is extracted through petroleum ether, and a petroleum ether layer is abandoned; the lower remaining solution is decompressed and concentrated to recycle a solvent, and extract of the extraction solution is obtained; after the extract is dissolved through the methyl alcohol, elution is carried out through a silicon gel chromatography column, chloroform and the methyl alcohol are in flowing phases, eluent is recycled, and TLC tracking detection is carried out; the obtained eluent with the cordycepin is decompressed and concentrated, and then is heated through proper methyl alcohol or ethyl alcohol to be dissolved, and low-temperature crystallization is carried out. The technology is easy and controllable, the extraction time is short, the consumption of the organic solvent is little, the organic solvent can be recycled, cost is low, and the obtained cordycepin is high in purity.

Description

technical field [0001] The invention relates to a method for extracting and purifying cordycepin, which belongs to the field of extraction and separation of effective components of medicinal fungi. Background technique [0002] Cordyceps militaris, also known as Cordyceps militaris, Cordyceps militaris, etc. Chinese medicine believes that Cordyceps is the only traditional Chinese medicine that can balance and regulate yin and yang. Kidney deficiency, impotence and nocturnal emission, soreness of waist and knees, weakness after illness, chronic cough and weakness, coughing up phlegm and blood due to labor, spontaneous sweating and night sweating, etc. Cordycepin is one of the main active ingredients of Cordyceps militaris. Modern pharmacological studies have shown that cordycepin has various functions such as inhibiting microbial growth, anti-tumor, regulating immunity, antibacterial, anti-inflammatory, anti-aging, improving metabolism, and scavenging free radicals. Pharmaco...

Claims

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Application Information

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IPC IPC(8): C07H19/16C07H1/08
CPCC07H1/08C07H19/16
Inventor 刘玉峰李胜男朱美霞韩彬王志萍卢晓丹
Owner 浙江中科宏寿医药科技有限公司
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