Extraction process of cordycepin (active substance) from silkworm pupa cordyceps militaris
A technology of active substances and extraction process, which is applied in the field of extraction process of active substances of traditional Chinese medicine, can solve problems such as difficult mass production, organic solvent pollution, special equipment, etc., and achieve the effects of short processing time, mild process conditions and extended storage period
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Embodiment 1
[0015] Weigh a certain amount of polyethylene glycol 6000 and dissolve it in deionized water, prepare the solution according to Table 1, and set aside. After drying at 65°C, silkworm fungus was placed in a fully enclosed powder equipment, and crushed at 25°C by means of mechanical extrusion and impact to emulsify the solid components. The crushed silkworm grass was weighed according to the ratio in Table 1. After fully dissolving with polyethylene glycol 6000 aqueous solution, add ammonium citrate to fully shake according to the ratio in Table 1, statically separate the phases, centrifuge, remove the precipitate to obtain the supernatant; the obtained supernatant is washed with ethyl acetate After being washed with petroleum ether, vacuum-dried to obtain cordycepin.
[0016]
Embodiment 2
[0017] Embodiment 2 extraction process compares
[0018] Cordyceps is dried at 65°C, placed in a fully enclosed powder equipment, crushed at 25°C by means of mechanical extrusion and impact to emulsify the solid components, and the crushed Cordyceps is extracted and purified according to the following different methods Cordycepin.
[0019] Sample 1 (reflux extraction-column chromatography purification) (refer to Chinese patent 00130376.7 for the method): take 400 parts of silkworm fungus, add 5 times the amount of 30% ethanol (temperature 70 ° C), soak for 48 hours, and put the soaked suspension on the Reflux device, heat and reflux for 2 hours, recover ethanol, add water to precipitate, adjust pH to 3.5, filter after 24 hours, dissolve the recovered medicinal solution with water and refrigerate and precipitate at 4°C for 24 hours. Filter the cold medicinal solution with a microporous membrane (0.85 μm) and adjust the filtrate to 4.0 with 0.1mol / L for later use, put on the io...
Embodiment 3
[0025] Embodiment 3 establishes the method for measuring cordycepin content
[0026] Chromatographic conditions Chromatographic column: Knauer Europher-100C18 (5μm, 4.6×250mm); mobile phase: acetonitrile-0.05mol / LKH 2 PO 4Buffer (7.5:92.5); flow rate: 1 mL / min detection wavelength: 260 nm; column temperature: 25°C; injection volume: 10 μL.
[0027] Selection of detection wavelength Take an appropriate amount of cordycepin reference substance, add methanol to make a solution containing 0.2 mg of cordycepin per 1 mL, and perform the determination according to the above-mentioned chromatographic conditions. It can be seen from the ultraviolet spectrum of the reference substance extracted that cordycepin has the maximum absorption at 259.3nm, so the final wavelength 260nm was selected for the determination of cordycepin.
[0028] Preparation of reference substance solution Take an appropriate amount of cordycepin reference substance dried at 105°C to constant weight, weigh it ac...
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