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Preparation method of high-purity plate-like cordycepin crystal

A high-purity technology for cordycepin, applied in the field of medicine and chemical industry, can solve the problems of high production cost, difficulty in large-scale industrial production, and the preparation method of high-purity sheet cordycepin crystals has never been reported, and achieves equipment investment and production and operation costs. Low, simple process effect

Inactive Publication Date: 2010-12-29
SHANGHAI GUOBAO ENTERPRISE DEV CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] According to all publicly reported patent documents on the separation and purification of cordycepin at home and abroad, the preparation method of high-purity flaky cordycepin crystals has never been reported
In the reported patent documents, the separation and purification process of cordycepin is relatively complicated, and it needs to be treated with different resins or need to use expensive high-performance liquid chromatography equipment. The production cost is high, and it is difficult to realize large-scale industrial production

Method used

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  • Preparation method of high-purity plate-like cordycepin crystal
  • Preparation method of high-purity plate-like cordycepin crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 24.89 kg of pulverized Cordyceps sinensis medium residue particles into a φ30×60cm stainless steel bucket with sealable ends, fill it evenly, without squeezing, and close the bucket tightly with a lid.

[0034] Use a diaphragm pump to pump 50 liters of drinking water from the bottom of the stainless steel barrel. The water extract from the upper end of the stainless steel barrel flows into a stainless steel column (φ10×120cm) containing 9 liters of H-20 macroporous resin from the lower end, and the upper end of the stainless steel column The effluent of the effluent is continuously pumped into the bottom of the stainless steel barrel with a diaphragm pump for water circulation extraction and adsorption at the same time; the opening time of the diaphragm pump, that is, the extraction time is 16h.

[0035] After extraction, 30 liters of 30% (V / V) ethanol aqueous solution was used as the eluent to elute the macroporous resin column with a flow rate of 1 BV / h; the eluent was...

Embodiment 2

[0039] Put 24.32 kg of pulverized Cordyceps militaris medium residue particles into a φ30×60cm stainless steel bucket with sealable ends. The filling should be even, without squeezing, and the bucket should be tightly closed with a lid.

[0040] Use a diaphragm pump to pump 50 liters of drinking water from the bottom of the stainless steel barrel. The water extract from the upper end of the stainless steel barrel flows into a stainless steel column (φ10×120cm) containing 9 liters of H-20 macroporous resin from the bottom. The upper end of the stainless steel column The effluent of the effluent is continuously pumped into the bottom of the stainless steel barrel with a high-pressure diaphragm pump for water circulation extraction. The opening time of the diaphragm pump, that is, the extraction time is 16h.

[0041] Use 30 liters of 20% (V / V) ethanol aqueous solution as the eluent, and use a diaphragm pump to pump the eluent into a stainless steel column equipped with macroporous resi...

Embodiment 3

[0045] Put 250 grams of the crushed Cordyceps militaris culture medium particles into a φ5.0×40cm PVC tube with sealable ends. The filling should be even, without squeezing, and the PVC tube should be tightly covered with a lid.

[0046] Use a peristaltic pump to pump 2500ml of drinking water from the bottom of the PVC pipe. The water extract from the upper end of the PVC pipe flows from the lower end into a glass column (φ2.5×50cm) filled with 100ml H-20 macroporous resin. The upper end of the glass column The effluent of the peristaltic pump is continuously pumped into the bottom end of the PVC pipe for water circulation extraction; the opening time of the peristaltic pump is 16 hours.

[0047] Use 400ml 30% (V / V) ethanol aqueous solution as the eluent, use a peristaltic pump to pump the eluent into a glass column with macroporous resin for elution, with a flow rate of 1BV / h; collect the eluent by rotary evaporation The instrument was concentrated under vacuum and reduced pressur...

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Abstract

The invention discloses a preparation method of high-purity plate-like cordycepin crystal. The method comprises the following steps: extracting cordycepin in a cordyceps militaris solid cultural medium residue, simultaneously enabling an extract to flow through macroporpous resin, and then carrying out recycling extraction and absorption on the cordyceps militaris solid cultural medium residue again; and eluting the cordycepin absorbed on the macroporpous resin, concentrating an eluent, crystallizing and recrystallizing to obtain the high-purity plate-like cordycepin crystal. The product obtained by the method has HPLC purity above 99.9% and is suitable for large-scale industrial production.

Description

[0001] technical field [0002] The invention relates to the field of medicine and chemical industry, in particular to a method for preparing high-purity flaky cordycepin crystals, in particular to a method for extracting high-purity flaky cordycepin crystals from culture medium residues of Cordyceps militaris. Background technique [0003] Cordyceps militaris (Cordyceps militaris), also known as Cordyceps militaris, belongs to Ascomycotina, Ergotaceae, Cordyceps, and is a precious medicinal fungus. In recent years, due to the increasing demand for natural Cordyceps sinensis and the depletion of limited resources, it has not yet been artificially cultivated on a large scale. So people began to cultivate Cordyceps militaris with a short production cycle and similar medical and health care effects with natural Cordyceps sinensis to meet consumer demand, replace the shortage of natural Cordyceps sinensis, and provide a broad market and good development opportunities for the dev...

Claims

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Application Information

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IPC IPC(8): C07H19/16C07H1/08
Inventor 唐永范唐亮
Owner SHANGHAI GUOBAO ENTERPRISE DEV CENT
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