Method for separating germacrone from Curcuma wenyujin volatile oil
A technology of gemmanone and volatile oil, applied in the field of traditional Chinese medicine pharmacy, can solve the problems of high cost, long time consumption of the target gemmanone, etc., and achieve the effects of simple operation, excellent separation effect and less solvent consumption.
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Embodiment 1
[0022] Prepare 0.1mol / L methyl-β-cyclodextrin aqueous solution and n-hexane in a volume ratio of 1:1, mix in a separatory funnel, shake fully, stand still, separate before use, the lower phase is selected as the stationary phase, and the upper phase Selected as the mobile phase; the column temperature is set at 20°C, first use a constant flow pump to inject the lower phase of the solvent system into the PTFE spiral tube of the HSCCC until the entire tube is filled, then turn on the HSCCC, rotate counterclockwise, and the speed At the same time, the mobile phase is pumped into the HSCCC separation column from the head end of the column at a flow rate of 2.0ml / min; when the mobile phase flows out from the end of the column, it indicates that the two phases in the HSCCC have reached equilibrium, and the sample is injected through the six-way valve HSCCC (536.4mg warm curcuma volatile oil sample is dissolved in the upper and lower phase solvents of 18ml equivolume mixing); Detect e...
Embodiment 2
[0024] Prepare 0.1mol / L methyl-β-cyclodextrin aqueous solution and n-hexane in a volume ratio of 1:1, mix in a separatory funnel, shake fully, stand still, separate before use, the lower phase is selected as the stationary phase, and the upper phase Selected as the mobile phase; the column temperature is set at 20°C, first use a constant flow pump to inject the lower phase of the solvent system into the PTFE spiral tube of the HSCCC until the entire tube is filled, then turn on the HSCCC, rotate counterclockwise, and the speed At the same time, the mobile phase is pumped into the HSCCC separation column from the head end of the column at a flow rate of 2.0ml / min; when the mobile phase flows out from the end of the column, it indicates that the two phases in the HSCCC have reached equilibrium, and the sample is injected through the six-way valve HSCCC (905.5mg warm curcuma volatile oil sample is dissolved in the upper and lower phase solvents of 18ml equivolume mixing); Detect e...
Embodiment 3
[0026] Prepare 0.05mol / L methyl-β-cyclodextrin aqueous solution and n-hexane at a volume ratio of 1:1, mix in a separatory funnel, shake fully, stand still, and separate before use. The lower phase is selected as the stationary phase, and the upper phase Selected as the mobile phase; the column temperature is set at 20°C, first use a constant flow pump to inject the lower phase of the solvent system into the PTFE spiral tube of the HSCCC until the entire tube is filled, then turn on the HSCCC, rotate counterclockwise, and the speed At the same time, the mobile phase is pumped into the HSCCC separation column from the head end of the column at a flow rate of 2.0ml / min; when the mobile phase flows out from the end of the column, it indicates that the two phases in the HSCCC have reached equilibrium, and the sample is injected through the six-way valve HSCCC (429.8mg turmeric volatile oil sample is dissolved in 18ml equal-volume mixed upper and lower phase solvents); image 3 Pea...
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