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Method for extracting and separating curdione from oil of zedoary turmeric

A technology of curcumedione and curcuma oil, applied in the separation/purification of carbonyl compounds, ion exchange, ion exchange regeneration, etc., can solve the problem of lack of high-purity curcumin.

Active Publication Date: 2012-05-23
HAINAN BIKAI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a high-purity monomer of curcumadione and a method for extracting and purifying curcumadione from zedoary oil, the monomer purity is as high as 99.9%, which solves the lack of high-purity curcumadione in the prior art The question of controls

Method used

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  • Method for extracting and separating curdione from oil of zedoary turmeric
  • Method for extracting and separating curdione from oil of zedoary turmeric
  • Method for extracting and separating curdione from oil of zedoary turmeric

Examples

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Embodiment 1

[0011] Take the chromatographic column and add 300 g of silica gel (dried at 105°C for 6 hours) for column chromatography to dry-pack the column, fill it up, vacuum pump for 6 hours, and use petroleum ether (60-90°C): ethyl acetate (18:1) to remove the chromatographic column. Column, take 30g of zedoary oil, add 15g of silica gel for column chromatography and mix well, put it on the column by dry method, use gradient elution method, and carry out gradient elution with petroleum ether (60-90°C) and ethyl acetate mixed solvent successively, wherein The volume ratio of petroleum ether: ethyl acetate is 100:0, 30:1, 25:1, 20:1, 15:1, 12:1, 9:1, and the eluate at each gradient is collected, each 30ml, immediately conduct TLC inspection on multiple eluents under each gradient to monitor the elution of curcumadione, and test results under the gradients of 12:1 and 9:1 show that multiple copies containing a single curcumadione spot The eluents were combined, concentrated, refrigerated...

Embodiment 2

[0013] Take the chromatographic column and add 300 g of silica gel (dry at 105°C for 6 hours) for column chromatography, dry fill the column, fill it up, vacuum pump for 6 hours, use petroleum ether (60-90°C): ethyl acetate (18:1) Go to the column, take 30g of zedoary oil, add 15g of silica gel for column chromatography and mix well, put it on the column by dry method, use gradient elution method, and sequentially use petroleum ether (60-90°C) and ethyl acetate mixed solvent for gradient elution, Wherein the volume ratio of petroleum ether:ethyl acetate is 100:0, 30:1, 25:1, 20:1, 15:1, 12:1, 9:1, and the eluate under each gradient is collected, 30ml of each fraction of the eluent was immediately checked by TLC to monitor the elution of curcumadione, and the detection results under the gradients of 12:1 and 9:1 showed that most of the eluents containing a single curcumadione spot The fractions of eluents were combined, concentrated, refrigerated at 0-2°C, and left for 48 hours...

Embodiment 3

[0015] Take the chromatographic column and add 600 g of silica gel (dried at 105°C for 6 hours) for column chromatography, fill the column with dry method, fill it up, vacuum pump for 6 hours, and use petroleum ether (60-90°C): ethyl acetate (18:1) Go to the column with ethyl acetate, take 60g of zedoary oil, add 30g of silica gel for column chromatography, mix well, put it on the column by dry method, use gradient elution method, and carry out gradient with petroleum ether (60-90°C) and ethyl acetate mixed solvent in sequence Elution, wherein the volume ratio of petroleum ether: ethyl acetate is 100:0, 30:1, 25:1, 20:1, 15:1, 12:1, 9:1, collect the elution under each gradient solution, 30ml each, immediately conduct TLC inspection on multiple eluents under each gradient to monitor the elution of curcumadione, and the detection results under the gradients of 12:1 and 9:1 show that there is a single curcumadione The multiple eluents from the spot were combined, concentrated, re...

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Abstract

The invention relates to a method for extracting and purifying curdione from the oil of zedoary turmeric, a natural medicinal plant volatile oil. The purity of the curdione obtained by the method reaches 99.9%, and the curdione conforms to the requirement of the purity of a contrast product in the field of traditional Chinese medicine and provides a superior raw material for developing a subsequent product. The method comprises the following steps: mixing the oil of the zedoary turmeric and silica gel used for chromatography evenly, coating a silica gel column, taking petroleum ether and ethyl acetate which have different proportions as an eluent for gradient elution, collecting and merging eluant containing the component of the curdione, concentrating, refrigerating, standing, precipitating crystals and separating and purifying the crystals again by the same method to obtain recrystallized crystals so as to obtain the curdione. The method features simple operation and good repeatability.

Description

technical field [0001] The invention relates to an extraction method for extracting a single effective component from volatile oil of natural medicinal plants, in particular to a method for extracting and purifying zedoary dione from zedoary oil, and the purity of zedoary dione prepared by the method is as high as 99.9%. Background technique [0002] Zedoary oil is a volatile oil extracted from various medicinal plants, such as turmeric, zedoary, turmeric and other Zingiberaceae plants contain zedoary oil. Zedoary oil contains a variety of active ingredients, which have the functions of promoting qi and blood circulation, eliminating accumulation and relieving pain, promoting blood circulation and removing blood stasis, removing putrefaction and promoting muscle growth, and enhancing the body's immunity. Modern pharmacological studies have shown that zedoary oil directly inhibits and destroys cancer cells; resists HPV infection; zedoary oil has a synergistic killing effect o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/607C07C45/79B01D15/08
Inventor 陈容史朝晖冯仲异
Owner HAINAN BIKAI PHARM CO LTD
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