Phyllanthostatin A preparation process
A preparation process and drying technology, which is applied in the field of preparation process of Phyllophyllum Stetin A, to achieve high separation efficiency and improve product purity
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Embodiment 1
[0012] Grind the dry roots of Acuminosa acuminata, pass through a 40-mesh sieve, take 5kg and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 38°C, the pressure is 25MPa, and CO 2 The flow rate is 18L / h. After the environment in the extraction tank is stable, 1500ml of 95% ethanol is introduced as an entrainer to participate in the extraction. After 2 hours of extraction, analysis is carried out at a temperature of 35°C and a pressure of 8.5MPa. The extract is collected from the separation tank and extracted The compound was repeatedly extracted with ether 4 times, and the ether extracts were combined and concentrated to obtain ether extract. Mix the ether extract with an appropriate amount of silica gel and mix well, use 5 times the amount of the extract to pack silica gel (column diameter to height ratio 1:10), put the mixed sample silica gel on the top of the co...
Embodiment 2
[0014] Grind the dry roots of Acuminosa acuminata, pass through a 40-mesh sieve, take 5kg and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 45°C, the pressure is 28MPa, and CO 2 The flow rate is 20L / h. After the environment in the extraction tank is stabilized, 750ml of 95% ethanol is introduced as an entrainer to participate in the extraction. After 3 hours of extraction, analysis is performed. The analysis temperature is 35°C and the pressure is 8.5MPa. The extract is collected from the separation tank and extracted The compound was repeatedly extracted with ether for 5 times, and the ether extracts were combined and concentrated to obtain ether extract. Mix the ether extract with an appropriate amount of silica gel and mix well, use 4 times the amount of silica gel to pack the extract into a column (column diameter to height ratio 1:8), put the mixed sample si...
Embodiment 3
[0016] Grind the dry roots of Acuminosa acuminata, pass through a 40-mesh sieve, take 5kg and put it into the extraction kettle, and pass it into supercritical CO 2 For extraction, set the parameters of the extraction kettle: the extraction temperature is 55°C, the pressure is 29MPa, and CO 2 The flow rate is 26L / h. After the environment in the extraction tank is stabilized, 1000ml of 95% ethanol is introduced as an entrainer to participate in the extraction. After 2.5 hours of extraction, analysis is performed. The analysis temperature is 40°C and the pressure is 9MPa. The extract is collected from the separation tank and extracted The compound was repeatedly extracted with ether 4 times, and the ether extracts were combined and concentrated to obtain ether extract. Mix the ether extract with an appropriate amount of silica gel and mix well, use silica gel 6 times the amount of the extract to pack the column (column diameter to height ratio 1:15), put the mixed sample silica ...
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