Method for preparing jolkinolide B

A technique of spurge lactone and ethyl acetate, which is applied in the field of natural medicinal chemistry, can solve the problems such as the mass production of spurge lactone, which has not yet been seen, and achieves the effects of overcoming the dead adsorption of samples, short preparation period and large preparation volume.

Inactive Publication Date: 2013-01-02
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There is no report on the method of preparing southern euphorlide B in large quantities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Get Euphorbia root and pulverize through 60 mesh, get 3kg of raw material and add supercritical CO 2 In the extraction kettle, turn on the equipment and adjust the equipment parameters: the extraction temperature is 56°C, the extraction pressure is 33.6MPa, the temperature of the separation kettle I is 45°C, and the pressure is 9MPa, the temperature of the separation kettle II is 37°C, and the pressure is 7MPa. into CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 20L / h, and 6L of 75% ethanol aqueous solution was entrained, and the dynamic extraction was performed for 4 hours. The extract was collected, ethanol was recovered, and heptane was added to degrease to obtain the extract. Take heptane, ethyl acetate, acetonitrile, and water, and mix them in a ratio of 4:5:3:1. Take the upper phase and pump it into the separation column until the separation column is filled with the stationary phase at a speed of 850 rpm. P...

Embodiment 2

[0017] Get Euphorbia root and pulverize through 40 mesh, get 5kg raw material and add supercritical CO 2 In the extraction kettle, turn on the equipment and adjust the equipment parameters: the extraction temperature is 49°C, the extraction pressure is 28MPa, the temperature of the separation kettle I is 40°C, the pressure is 10MPa, the temperature of the separation kettle II is 32°C, and the pressure is 7MPa. into CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 16L / h, and 8L of 75% ethanol aqueous solution was entrained, and the dynamic extraction was performed for 3 hours. The extract was collected to recover ethanol, and heptane was added to degrease to obtain the extract. Take heptane, ethyl acetate, acetonitrile, and water, and mix them in a ratio of 7:3:4:2. Take the upper phase and pump it into the separation column until the separation column is filled with the stationary phase at a speed of 700 rpm. Pump in at a ...

Embodiment 3

[0019] Take Euphorbia root and crush it through 60 mesh, take 10kg of raw material and add supercritical CO 2 In the extraction kettle, turn on the equipment and adjust the equipment parameters: the extraction temperature is 43°C, the extraction pressure is 25MPa, the temperature of the separation kettle I is 35°C, and the pressure is 8MPa, the temperature of the separation kettle II is 25°C, and the pressure is 4MPa. into CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 15L / h, and entrained with 10L of 75% ethanol aqueous solution, extracted dynamically for 2 hours, collected the extract, recovered 75% ethanol aqueous solution, added heptane to degrease, and obtained the extract. Take heptane, ethyl acetate, acetonitrile, and water, and mix them in a ratio of 5:2:3:2. Take the upper phase and pump it into the separation column until the separation column is filled with the stationary phase at a speed of 900 rpm. Pump in a...

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PUM

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Abstract

The invention belongs to the field of natural pharmaceutical chemistry and relates to a method for preparing jolkinolide B. The method comprises the following steps: taking euphorbia jolkini roots, crushing, screening by a sieve with 40-60 meshes, feeding the euphorbia jolkini roots to an extraction kettle, carrying out supercritical co2 extraction by using ethanol water solution with the volume percentage of 75% as an entrainer, collecting extract liquid, degreasing with heptane after recovering ethanol, carrying out high-speed counter-current chromatography by using heptane-ethyl acetate-acetonitrile-water as a solvent system and drying the fraction to obtain the jolkinolide B. Jolkinolide B products prepared by the method have the advantages of having no pollution and high yield, and the method is suitable for industrial preparation of jolkinolide B.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a method using supercritical CO 2 A method for preparing southern euphoride B by extraction and high-speed countercurrent chromatographic separation techniques. Background technique [0002] Southern Euphorbialide B is a diterpenoid compound, mp.212°C (decomposition), white needle crystal, molecular formula C 20 h 26 o 4 , molecular weight 330.42. Southern Euphorbialide B widely exists in natural plants and is mainly isolated from Euphorbiaceae plants. Pharmacological studies have shown that southern euphorbialide B has the effect of promoting the formation of nerve growth factors, and can be used to treat spinal injuries, peripheral nerve injuries, diabetic neuropathy and lateral sclerosis of muscle atrophy. In addition, it also has anti-cancer activity. The anti-cancer activity test in animals shows that Euphorlide B has the obvious activity of inhibiting the gro...

Claims

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Application Information

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IPC IPC(8): C07D493/20
CPCY02P20/54Y02P20/582
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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