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Method for separating and purifying 6-gingerol by reduced pressure column chromatography and production method of 6-gingerol

A technology of separation and purification and decompression column, which is applied in the field of separation and purification, can solve the problems of seldom mentioning the recovery rate of 6-gingerol, increase the complexity of the separation process, consume large raw materials, etc., and achieve short elution time, fewer types, The effect of less consumption

Active Publication Date: 2019-03-22
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the combination of multiple separation technologies will increase the complexity of the separation process and increase the cost.
In order to obtain milligram-level 6-gingerol, it often takes a lot of raw materials, so the recovery rate of 6-gingerol after separation and purification is rarely mentioned in many studies on gingerol

Method used

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  • Method for separating and purifying 6-gingerol by reduced pressure column chromatography and production method of 6-gingerol
  • Method for separating and purifying 6-gingerol by reduced pressure column chromatography and production method of 6-gingerol
  • Method for separating and purifying 6-gingerol by reduced pressure column chromatography and production method of 6-gingerol

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Embodiment 1

[0089] The present embodiment provides a method for separating and purifying 6-gingerol by column chromatography under reduced pressure, which comprises the following steps:

[0090] S100, the first step decompression gradient chromatography column

[0091] Completely dissolve the raw material containing 6-gingerol with ethyl acetate, add sample mixing silica gel, volatilize and remove the ethyl acetate, use 300-400 mesh chromatography silica gel to dry-pack the column, and combine the raw material containing 6-gingerol with the first subtraction The mass ratio of silica gel in the pressure column is 1:100. Use the first mixed solvent with different ratios of n-hexane-ethyl acetate as the mobile phase for gradient elution in the first decompression column. The densities of the first mixed solvent are 0.670g / ml, 0.676g / ml, and 0.682g / ml respectively , 0.687g / ml; the eluent was identified by thin-layer chromatography, compared with 6-gingerol standard substance, and the develop...

Embodiment 2

[0095] The present embodiment provides a method for separating and purifying 6-gingerol by column chromatography under reduced pressure, which comprises the following steps:

[0096] S100, the first step decompression gradient chromatography column

[0097] Completely dissolve the raw material containing 6-gingerol with ethyl acetate, add sample mixing silica gel, volatilize and remove the ethyl acetate, use 300-400 mesh chromatography silica gel to dry-pack the column, and combine the raw material containing 6-gingerol with the first subtraction The mass ratio of silica gel in the pressure column is 1:110. Use the first mixed solvent with different ratios of n-hexane-ethyl acetate as the mobile phase for gradient elution in the first decompression column. The densities of the first mixed solvent are 0.673g / ml, 0.678g / ml, and 0.684g / ml respectively , 0.689g / ml; the eluent was identified by thin-layer chromatography, compared with 6-gingerol standard substance, and the develop...

Embodiment 3

[0101] The present embodiment provides a method for separating and purifying 6-gingerol by reduced pressure column chromatography, which comprises the following steps:

[0102] S100, the first step decompression gradient chromatography column

[0103] The raw material containing 6-gingerol was completely dissolved in ethyl acetate, the mixed silica gel was added, the ethyl acetate was removed by volatilization, and 300-400 mesh chromatographic silica gel was used for dry packing. The mass ratio of silica gel in the pressure column is 1:100. Use the first mixed solvent with different ratios of n-hexane-ethyl acetate in the first reduced pressure column to elute gradiently, the density and dosage of the first mixed solvent are 0.670g / ml, 0.677g / ml, 0.683g respectively / ml, 0.688g / ml; the eluent was identified by thin-layer chromatography, compared with 6-gingerol standard, and the developing solvent was n-hexane and ethyl acetate with a volume ratio of 2:1. The same parts were...

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Abstract

The invention relates to the fields of separation and purification and provides a method for separating and purifying 6-gingerol by reduced pressure column chromatography and a production method of the 6-gingerol. The method for separating and purifying the 6-gingerol by the reduced pressure column chromatography comprises the following steps: performing gradient elution on a raw material containing the 6-gingerol through a first mixed solvent with N-hexane-ethyl acetate as a mobile phase in different proportions to obtain a 6-gingerol crude product; and performing gradient elution on the 6-gingerol crude product in a second reduced pressure column through a second mixed solvent with N-hexane-ethyl acetate as a mobile phase in different proportions to obtain a 6-gingerol purified substance. The method for separating and purifying the 6-gingerol by the reduced pressure column chromatography and the production method of the 6-gingerol, provided by the invention, have the benefits that the 6-gingerol is separated and purified by utilizing a two-step reduced pressure gradient elution method; through the reduced pressure operation, the operation is easier to control, and the elution time is short; meanwhile, the N-hexane-ethyl acetate mixed in different proportions is adopted as the mobile phase, the mobile phase is few in types, the consumption is less, and the recovery is easy.

Description

technical field [0001] The invention relates to the field of separation and purification, in particular to a method for separating and purifying 6-gingerol by reduced pressure column chromatography and a method for producing 6-gingerol. Background technique [0002] Gingerol is a kind of spicy substance naturally present in ginger. It is a yellow oily liquid. It is also the main active ingredient of gingerol. It is a compound composed of alkyl chain homologues containing β-hydroxy ketone structure. Gingerol is a class of compounds, mainly including more than ten components such as 4-gingerol, 6-gingerol, 8-gingerol, 10-gingerol and 12-gingerol. More than 75% of phenolic substances, and more than 80% of total gingerols in fresh ginger. 6-gingerol has the highest content among gingerols, and has a variety of biological activities, such as antioxidant, anti-mutagenic, anti-inflammatory, anti-rheumatic, anti-tumor, expelling cold, protecting liver and gallbladder. [0003] The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/42C07C49/255C07C45/78
CPCB01D15/426C07C45/78C07C49/255
Inventor 余德顺马龙利陈可可叶菲菲李岗于海
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI
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