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.

Active Publication Date: 2016-01-13
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The general countercurrent chromatographic separation method takes a long time and costs a lot to obtain the target gemmacone

Method used

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  • Method for separating germacrone from Curcuma wenyujin volatile oil
  • Method for separating germacrone from Curcuma wenyujin volatile oil
  • Method for separating germacrone from Curcuma wenyujin volatile oil

Examples

Experimental program
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Effect test

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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Abstract

The invention discloses a method for separating germacrone from Curcuma wenyujin volatile oil. The method comprises the following steps: fully mixing an aqueous solution of methyl-beta-cyclodextrin with n-hexane according to a volume ratio of 1:0.5-2, standing, carrying out liquid separation to respectively obtain an upper phase which is a mobile phase and a lower phase which is the stationary phase of a high-speed countercurrent chromatograph; and weighing the Curcuma wenyujin volatile oil, dissolving the Curcuma wenyujin volatile oil in a mixture containing the upper phase and the lower phase according to a volume ratio of 1:1, introducing the above obtained sample, carrying out high-speed countercurrent chromatographic separation, detecting through an ultraviolet detector, collecting corresponding effluents corresponding to peaks in the spectrogram of the ultraviolet detector, concentrating germacrone-containing effluents, and drying to prepare pure germacrone. The method has the advantages of simple operation, less solvent consumption, high efficiency, fastness, strong purposefulness and good separation effect.

Description

(1) Technical field [0001] The invention belongs to the field of traditional Chinese medicine pharmacy, and relates to a method for separating gemmacone from the volatile oil of turmeric curcuma rich in gemmacone. (2) Technical background [0002] Gemacone is a monocyclic sesquiterpene compound present in the volatile oil of turmeric, which is used for relieving asthma and relieving cough, and inhibiting the proliferation of liver cancer BEL7402 cells. Gemacrone, the English name is germacrone, molecular formula C 15 h 22 O, molecular weight 218.33, molecular structure is as follows: [0003] [0004] Wen Yujin has the effects of promoting qi and dispelling fatigue, clearing heart-fire and relieving stagnation, promoting gallbladder and reducing jaundice. It is mainly used to treat amenorrhea, dysmenorrhea, abdominal distension pain, tingling pain, fever, dysentery, jaundice and red urine. At present, the extraction of gemmaconone is mainly eluted by silica gel column ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/647C07C45/78
CPCC07C45/78C07C49/647
Inventor 童胜强鲁梦霞颜继忠
Owner ZHEJIANG UNIV OF TECH
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