Supercritical CO2 extraction process of total rhubarb anthraquinone
A carbon dioxide and supercritical technology, applied in the direction of hydrocarbon production from carbon oxides, organic chemistry, quinone separation/purification, etc., can solve the problems that there is no supercritical carbon dioxide extraction of total anthraquinone extract of rhubarb, and avoid high temperature hydrolysis , less pollution and shorter extraction time
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Embodiment 1
[0021] Weigh 1.5 kg of rhubarb medicinal material powder, spray and infiltrate with 300 ml of 50% ethanol, and after airtight and stuffy for 0.5 hours, put it into a 5 L specification supercritical extraction device extraction kettle, use supercritical carbon dioxide as the extraction solvent, and the extraction process is carried out at a pressure of 20Mpa, temperature is 30 ℃, the time is to carry out in the environment of 0.5 hour, in the whole extraction process, with the 300ml concentration of 5 milliliters / minute flow rate, be that the ethanol of 60% extracts as entrainer and solvent; Under reduced pressure analysis and separation at ℃, collect about 550ml of ethanol solution of rhubarb total anthraquinones, concentrate and dry under reduced pressure to obtain 30.0 g of its extract, the sample yield is 2.00%, and the content of total anthraquinones in the sample is 32.5%.
Embodiment 2
[0023] Weigh 1.5 kg of rhubarb medicinal material powder, spray and infiltrate with 300 ml of 95% ethanol, and after airtight and stuffy for 3 hours, put it into a 5 L specification supercritical extraction device extraction kettle, use supercritical carbon dioxide as the extraction solvent, and the extraction process is carried out at a pressure of 35Mpa, temperature is 50 ℃, the time is to carry out in the environment of 2 hours, in the whole extraction process, with the concentration of 3 milliliters / min of 500ml flow rate, be that the ethanol of 95% extracts as entrainer and solvent; Under reduced pressure analysis and separation at 25°C, about 800ml of ethanol solution of rhubarb total anthraquinones was collected, concentrated and dried under reduced pressure to obtain 32.1g of its extract, the sample yield was 2.14%, and the total anthraquinone content in the sample was 36.4%.
Embodiment 3
[0025] Weigh 1.5kg of rhubarb medicinal material and grind it into fine powder, spray it with 300ml of absolute ethanol for infiltration, seal it for 1 hour, put it into a 5L supercritical extraction device extraction kettle, and use supercritical carbon dioxide as the extraction solvent. Pressure is 30Mpa, temperature is 40 ℃, the time is carried out in the environment of 3 hours, in the whole extraction process, with the concentration of 2 milliliters / minute with 750ml flow velocity, be that the ethanol of 90% extracts as entrainer and solvent; Under reduced pressure analysis and separation at a temperature of 30°C, about 1000ml of the ethanol solution of rhubarb total anthraquinones was collected, concentrated and dried under reduced pressure to obtain 38.0g of its extract, the sample yield was 2.53%, and the content of total anthraquinones in the sample was 31.5% %.
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