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Separation and purification method and production method of 6-gingerol

A technology for separation and purification of gingerol, applied in the field of separation and purification of 6-gingerol, can solve the problems of difficulty in mass-scale preparation and production, decrease in separation efficiency, decrease in yield and the like, and achieve easy scale-up of mass production and consumption of organic solvents. Small, simple process effects

Active Publication Date: 2019-03-29
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Ginger oil or ginger oleoresin containing 6-gingerol, wherein the further purification of 6-gingerol usually requires multiple column chromatography and macroporous resin column chromatography or high-speed countercurrent chromatography. The disadvantages of recrystallization after analysis are as follows: 1. Multiple column chromatography takes a long time and consumes a lot of organic solvents; 2. Multiple column chromatography needs to use different specifications of separation packing, and the number of uses is limited, and the packing after recycling and reprocessing 3. The loss of 6-gingerol will be caused while passing through the column continuously, resulting in a decrease in yield; 4. In the multiple column chromatography technology, the separation period of the normal pressure column is slow and the period of pressurization and decompression is long. The pressure column has requirements for its column, and its size and specification have a great impact on the technical parameters and separation efficiency of the scale-up process, which leads to the instability of the scale-up batch production process and limits the application of column chromatography technology in the actual batch scale-up production process;5 .High-speed countercurrent chromatography requires special equipment and equipment, which is not easy to scale up and expensive equipment; 6. The recrystallization method is suitable for improving the purity of high-purity substances, and it is also difficult to prepare and produce in batches

Method used

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Examples

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Effect test

Embodiment 1

[0029] The present embodiment provides a kind of separation and purification method of 6-gingerol, it comprises the following steps:

[0030] The 6-gingerol content that obtains with organic solvent method is in 10% ginger oil and ginger oleoresin as raw material, with 23 times (v / m) n-hexane-ethyl acetate (v / v, n-hexane 70%) Dissolve the above raw materials under appropriate heating (40°C) and stirring, and separate the n-hexane-ethyl acetate layer and insoluble matter after standing still.

[0031] Use 50 times (v / v) of methanol-water (v / v, methanol 40%) to carry out liquid-liquid extraction and separation operation for the n-hexane-ethyl acetate layer. The extraction temperature is not lower than room temperature. After the extraction is completed, let it stand for a period of time. Separation of incompatible two phases; this liquid-liquid extraction separation operation step is repeated 3 times, the methanol-water phase is combined each time, and the n-hexane layer and the...

Embodiment 2

[0033] The present embodiment provides a kind of separation and purification method of 6-gingerol, it comprises the following steps:

[0034] supercritical CO 2 The 6-gingerol content that extraction method obtains is in 20% ginger oil and ginger oleoresin as raw material, with 20 times of (v / m) n-hexane-ethyl acetate (v / v, n-hexane 50%) in appropriate addition Warm (50°C) and stirring to dissolve the above raw materials, after standing still, separate the n-hexane-ethyl acetate layer and insoluble matter.

[0035] The n-hexane-ethyl acetate layer uses 30 times (v / v) methanol for liquid-liquid extraction and separation operation. The extraction temperature is not lower than room temperature. After the extraction is completed, let it stand for a while to separate the incompatible two phases; The separation operation steps are repeated 4 times, each time methanol is combined, and the n-hexane layer and the combined methanol are subjected to vacuum distillation to recover reusab...

Embodiment 3

[0037] The present embodiment provides a kind of separation and purification method of 6-gingerol, it comprises the following steps:

[0038] The 6-gingerol content that obtains with organic solvent method is in 10%-30% ginger oil and ginger oleoresin as raw material, with 10 times (v / m) normal hexane-ethyl acetate (v / v, normal hexane 90%) to dissolve the above raw materials under proper heating (60° C.) and stirring, and separate the n-hexane-ethyl acetate layer and insoluble matter after standing still.

[0039] Use 100 times (v / v) ethanol-water (v / v, ethanol 40%) to carry out liquid-liquid extraction and separation operation for the n-hexane-ethyl acetate layer. The extraction temperature is not lower than room temperature. After the extraction is completed, let it stand for a period of time. Separation of incompatible two phases; this liquid-liquid extraction separation operation step is repeated 3 times, each time the ethanol-water phase is combined, and the n-hexane laye...

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Abstract

The invention relates to the field of separation and purification, and provides a separation and purification method and a production method of 6-gingerol. The separation and purification method of the 6-gingerol comprises the following steps of: dissolving a raw material containing the 6-gingerol into a first organic solvent, and then carrying out liquid-liquid extraction separation on the firstorganic solvent in which the raw material containing the 6-gingerol is dissolved by using a second organic solvent which is insoluble in the first organic solvent. The production method of the 6-gingerol comprises an extracting method of the 6-gingerol and the separation and purification method of the 6-gingerol. According to the separation and purification method of the 6-gingerol, provided by the embodiment of the invention, the 6-gingerol can be quickly separated and purified through liquid-liquid extraction, e consumed time is short, the organic solvents can be recycled, a separation and purification process is simple, the required equipment is conventional equipment, the yield is high, and large-batch production is easy. According to the production method of the 6-gingerol, provided by the embodiment of the invention, the 6-gingerol obtained through extraction, separation and purification has the advantages of high content, higher yield, shorter consumed time and less organic solvent consumption.

Description

technical field [0001] The invention relates to the field of separation and purification, in particular to a separation and purification method and production method of 6-gingerol. Background technique [0002] The separation and purification methods of 6-gingerol mainly include silica gel column chromatography, macroporous adsorption resin method, polyamide column separation method, molecular distillation technology, preparative high-performance liquid chromatography and high-speed countercurrent chromatography, etc. At present, among the separation methods of 6-gingerol, column chromatography is the most widely used and mature method. [0003] Ginger oil or ginger oleoresin containing 6-gingerol, wherein the further purification of 6-gingerol usually requires multiple column chromatography and macroporous resin column chromatography or high-speed countercurrent chromatography. The disadvantages of recrystallization after analysis are as follows: 1. Multiple column chromat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/255C07C45/80
CPCC07C45/80C07C49/255Y02P20/54
Inventor 余德顺马龙利陈可可
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI
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