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Method for separating and purifying 6-gingerol

A technology for separation and purification of gingerol, applied in the field of natural medicine, can solve the problems of long operation time, expensive packing, low separation efficiency, etc., and achieve the effects of good quality of finished products, easy operation and high output

Active Publication Date: 2007-07-11
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 6-gingerol has unstable physical and chemical properties due to its 8-hydroxyketone structure in its molecule, and it coexists with a variety of chemical components with similar structures, making it difficult to separate
The packing material used in Sephadex LH 20 column chromatography is expensive, the operation time is long, the separation efficiency is low, and it is not suitable for large-scale applications
In addition, the literature does not specify the final n-hexane recrystallization step
It has been proved by experiments that 6-gingerol does not dissolve well in n-hexane under the condition of only heating
[0006] Obviously, due to the constraints of cost and output, it is still difficult to realize the pharmacological research and quality control of ginger traditional Chinese medicine based on 6-gingerol.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preliminary separation by silica gel column chromatography

[0034] Use 300g of commercial ginger supercritical fluid extract as raw material, mix the sample with 200g of 100-200 mesh column chromatography silica gel, use 100-200 mesh column chromatography with 2kg of silica gel as the stationary phase, gradient elution, and the polarity of the eluents in sequence Petroleum ether: ethyl acetate = 12: 1, petroleum ether: ethyl acetate = 9: 1 and petroleum ether: ethyl acetate = 6: 1, collected petroleum ether: ethyl acetate = 6: 1 fraction, TLC test combined , and evaporated to dryness on a rotary evaporator to obtain 16.5 g of crude 6-gingerol, with a yield of 5.5%. Its purity is above 65% (HPLC test, area normalization method).

[0035] (2) Refined by silica gel column chromatography

[0036] Mix the 6-gingerol crude product obtained in the previous step, use 200-300 mesh chromatography silica gel as the stationary phase, the amount of silica gel used is 20 times...

Embodiment 2

[0043] (1) Preliminary separation by silica gel column chromatography

[0044]Using 250g of commercial ginger supercritical fluid extract as raw material, 200g of 100-200 mesh column chromatography silica gel as a sample, 1.5kg of 100-200 mesh column chromatography silica gel as a stationary phase, gradient elution, and the polarity of the eluent Petroleum ether: ethyl acetate = 12:1, petroleum ether: ethyl acetate = 9:1 and petroleum ether: ethyl acetate = 6:1, collected petroleum ether: ethyl acetate = 6:1, TLC inspection Combined and evaporated to dryness on a rotary evaporator to obtain about 12 g of crude 6-gingerol with a yield of 4.8%. Its purity is above 65% (HPLC test, area normalization method).

[0045] (2) Refined by silica gel column chromatography

[0046] Mix the 6-gingerol crude product obtained in the previous step, use 200-300 mesh chromatography silica gel as the stationary phase, the amount of silica gel used is 15 times that of the 6-gingerol crude produ...

Embodiment 3

[0053] (1) Preliminary separation by silica gel column chromatography

[0054] Use commercial ginger supercritical fluid extract 100g as raw material, mix sample with 60g silica gel for 100-200 mesh column chromatography, use 1.0kg silica gel for column chromatography with 100-200 mesh as stationary phase, gradient elution, eluent polarity Petroleum ether: ethyl acetate = 12:1, petroleum ether: ethyl acetate = 9:1 and petroleum ether: ethyl acetate = 6:1, collected petroleum ether: ethyl acetate = 6:1, TLC inspection Combined and evaporated to dryness on a rotary evaporator to obtain the crude product of 6-gingerol. It is about 6.5g, the yield is 6.5%, and its purity is above 65% (HPLC test, area normalization method).

[0055] (2) Preparative HPLC purification

[0056] Dissolve the crude 6-gingerol obtained in the previous step with an appropriate amount of methanol, filter it through a 0.45 μm microporous membrane, and purify it by HPLC using Angilent 1100 series. The mobi...

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PUM

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Abstract

The invention discloses a separating method of 6-gingerol, which is characterized by the following: adopting multiple chromatographic ways to separate effective component 6-gingerol in the traditional Chinese medicine ginger; accelerating the separating course; simplifying the operation; improving the quality and production.

Description

technical field [0001] The invention relates to the field of natural medicines, in particular to a method for separating the active ingredient 6-gingerol, that is, a method for separating the active ingredient 6-gingerol in the traditional Chinese medicine ginger by using multiple chromatographic means in orderly combination. Background technique [0002] Ginger and dried ginger are the fresh rhizome and dried rhizome of Zingiber officinale Rosc., which are commonly used in traditional Chinese medicine. The main components in ginger are volatile oil components, gingerol components and diphenylheptane components. Among them, gingerol has a large content of components, has obvious spicy taste and biological activity, and has been confirmed by modern research to have various pharmacological activities, which can be used as the research basis for the pharmacological activity and quality control of ginger and dried ginger. There are many kinds of gingerol components, among which...

Claims

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Application Information

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IPC IPC(8): C07C49/255C07C45/78
Inventor 李萍王伟李沁楚楚
Owner CHINA PHARM UNIV
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