Method and device for preparing highly-pure capsicum pigment capsaicin through supercritical fluid column chromatography

A technology for supercritical fluid and capsaicin, which is applied in the field of supercritical fluid column chromatography to separate and prepare high-purity natural products, and in the field of supercritical fluid preparative chromatography, which can solve unseen problems.

Inactive Publication Date: 2017-09-15
GUANGZHOU LEADER BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is also no related invention of supercritical fluid chromatography separation system with industrial feasibility collection separation system and tail gas recovery circulation system

Method used

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  • Method and device for preparing highly-pure capsicum pigment capsaicin through supercritical fluid column chromatography
  • Method and device for preparing highly-pure capsicum pigment capsaicin through supercritical fluid column chromatography
  • Method and device for preparing highly-pure capsicum pigment capsaicin through supercritical fluid column chromatography

Examples

Experimental program
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Embodiment 1

[0062] The pigment pepper extract produced by parallel organic solvent countercurrent extraction is used as raw material, and various pigment compounds are extracted and separated from it. The total capsaicin content in the raw material is 0.08%, and the color value is 235. The filter column is filled with 20 μm silica gel with a diameter of 100 mm and a column length of 200 mm. The separation column is filled with 50 μm silica gel with a diameter of 200 mm and a column length of 1800 mm. The adsorption column packing is activated carbon. The composition of fractions was monitored by an online ultraviolet detector, and the detection wavelength was set at 460 nm. The feeding tank is equipped with a preheating system, and the chromatographic column is equipped with a temperature control and balance system.

[0063] A single-channel batch supercritical chromatographic preparation process is used.

[0064] This example mainly prepares solvent-free high-purity pigment compounds....

Embodiment 2

[0074] The capsicum crude extract (capsaicin content 10%, color value 62) that 20Kg horizontal rotation extractor countercurrent extraction obtains is mixed with 20Kg50% ethanol / water, it is heated and saponified with 4Kg10% sodium hydroxide, and saponification temperature is controlled at 40-60°C, after saponification for 1-2h, cool and stand still, and separate and obtain 2.6Kg of saponified product in the upper layer. With this saponification product as raw material, a dual-channel supercritical fluid column chromatography preparation system ( figure 2 ) Continuously prepare high-purity capsaicin and capsaicin.

[0075] Put 1Kg of the saponification product above into a group of batch feeding tanks, the chromatographic column filler is 50 μm silica gel particles, and the adsorption column filler is activated carbon. Adjust the temperature of the feeding tank to 32°C, and increase the pressure to 28MPa. The raw material is dissolved and carried into the chromatographic col...

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Abstract

The invention relates to a method and a device for preparing a highly-pure capsicum pigment capsaicin through supercritical fluid column chromatography. The method comprises the following steps: mixing and dissolving supercritical carbon dioxide or modified supercritical carbon dioxide and capsicum oleoresin or saponification products thereof in a feeding tank, filtering the obtained solution, carrying out adsorption and desorption separation through a preparative chromatography column filled with solid adsorbent particles, collecting an eluate containing different solutes to corresponding collectors according to the signal of a detector, separating the solute components and carbon dioxide in a separator, carrying out filtering dedusting, condensation liquid removal, adsorption column purification and compression on tail gas to form a liquid, and returning the liquid to a storage tank in order to carry out cycle use. Extremely low solvent residual and even no solvent residual products with a high purity, such as capsanthin, capsorubin, beta-carotene, beta-cryptoxanthin, zeaxanthine, capsanthin ester, capsorubin ester and cryptoxanthin ester, and highly pure products, such as nordihydrocapsaicin, capsaicin and dihydrocapsaicin can be prepared through the method.

Description

technical field [0001] The invention relates to supercritical fluid preparation chromatographic technology, in particular to a process for preparing high-purity natural products by using supercritical fluid column chromatography, and belongs to the field of natural product purification and preparation. Background technique [0002] Supercritical fluid column chromatography, also called supercritical fluid column chromatography, is a chromatographic column separation technology that uses supercritical fluid as the mobile phase and solid particulate adsorbent as the stationary phase. Supercritical fluid has a density similar to that of a liquid and a solvating force similar to an organic solvent, and its diffusion coefficient is 1-2 orders of magnitude higher than that of a liquid. Near the critical temperature, small changes in pressure can cause large changes in density. The change of density significantly affects the dissolving ability of supercritical fluid, so by changin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B61/00C07C403/24C07C231/24C07C233/20C07C233/18C07D307/62B01D15/10
CPCB01D15/10C07C231/24C07C233/18C07C233/20C07C403/24C07D307/62C09B61/00Y02P20/54
Inventor 林劲冬黄俊霖陶正国朱熇崔海滨冼啟志
Owner GUANGZHOU LEADER BIO TECH
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