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Method for preparing high-purity bakuchiol through high-speed countercurrent chromatography separation

A high-speed countercurrent chromatography, bakuchiol technology, applied in chemical instruments and methods, organic compound preparation, organic chemistry and other directions, can solve the problem of polyamide column column efficiency decline, low bakuchiol extraction rate, and there will be samples and other problems, to achieve the effect of large preparation volume, good environmental protection function, and no sample loss

Pending Publication Date: 2021-07-27
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: a) the extraction rate of bakuchiol in psoralen medicinal material is low; b) polyamide column is a solid carrier, and there will be adsorption of samples, which will cause the column efficiency of polyamide column to continuously decline and the loss of samples

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Soaking the psoralen medicinal material in 95wt% ethanol solution at room temperature, extracting with high-speed stirring at room temperature in a reaction kettle, removing the 95wt% ethanol solution, and obtaining crude psoraleae extract. Mix n-hexane, methanol, and water at a volume ratio of 5:5:1 to prepare a solvent system, add it to a separatory funnel, shake it well, let stand to separate the phases, and obtain a two-phase mixed liquid, and collect the upper phase and the lower phase separately Solvent, respectively placed in an ultrasonic oscillator for ultrasonic degassing treatment, the crude psoraleae extract was dissolved in the upper phase solvent, and high-speed countercurrent chromatography was used for separation: the upper phase was the stationary phase, and the lower phase was the mobile phase, to further The completion of the sample is 0min, and the mixed solution of bakuchiol and the lower phase is obtained in 55-70min; the chromatographic conditions ...

Embodiment 2

[0023] Soaking the psoralen medicinal material in 95wt% ethanol solution at room temperature, extracting with high-speed stirring at room temperature in a reaction kettle, removing the 95wt% ethanol solution, and obtaining crude psoraleae extract. Mix n-heptane, ethanol, and water at a volume ratio of 5:5:2 to prepare a solvent system, add it to a separatory funnel, shake it well, let stand to separate the phases, and obtain a two-phase mixture, collect the upper phase and the lower phase separately Phase solvent, respectively placed in an ultrasonic oscillator for ultrasonic degassing treatment, the crude psoralen extract was dissolved in the upper phase solvent, and high-speed countercurrent chromatography was used for separation: the upper phase was the stationary phase, the lower phase was the mobile phase, and the The sample injection is 0 min, and the mixture of bakuchiol and the lower phase is obtained in 40-50 min; the chromatographic conditions are set as follows: the ...

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Abstract

The invention relates to a method for preparing high-purity bakuchiol by high-speed countercurrent chromatography separation. The method comprises the following steps: soaking a fructus psoraleae medicinal material in an ethanol solution, and extracting to obtain a fructus psoraleae crude extract; fully shaking the solvent system, standing for phase splitting, and separately collecting an upper phase and a lower phase; dissolving the fructus psoraleae crude extract in the upper phase, separating by adopting high-speed counter-current chromatography to obtain a mixed solution of bakuchiol and a lower phase by taking the upper phase as a stationary phase and the lower phase as a mobile phase, and removing the lower phase to obtain bakuchiol. According to the method, the high-purity bakuchiol is separated and purified from the fructus psoraleae medicinal material by utilizing a high-speed counter-current chromatography technology for the first time, all reagents of a solvent system can be recycled, and a good environment-friendly function is achieved.

Description

technical field [0001] The invention belongs to the technical field of cosmetic raw material processing, and in particular relates to a method for preparing high-purity bakuchiol through high-speed countercurrent chromatographic separation. Background technique [0002] Psoralen is the dry ripe fruit of Psoralea corylifolia L., a leguminous plant. Bakuchiol is an important monoterpene compound in psoralen, which has various pharmacological activities such as whitening, antibacterial, anti-inflammatory, anti-aging, and anti-oxidation. How to prepare high-purity bakuchiol in a large amount simply and quickly is a problem closely watched in the industrial production as a cosmetic raw material. [0003] Patent CN108299453A discloses a method for separating psoralen, isopsoralen and bakuchiol from psoralen, comprising the following steps: a) extracting the psoralen medicinal material with petroleum ether after crushing to obtain The petroleum ether crude extract of psoralen; b)...

Claims

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Application Information

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IPC IPC(8): C07C39/19C07C37/82
CPCC07C37/82C07C39/19
Inventor 余琦邓力
Owner SHANGHAI TAUTO BIOTECH CO LTD
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