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Method for preparing Wikstroelide D

A technology of kelp ester and kelp flower, applied in the field of natural medicinal chemistry, to achieve the effect of overcoming dead adsorption of samples, large amount of preparation, and short preparation cycle

Inactive Publication Date: 2013-01-09
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no domestic report on the method of preparing a large amount of fennelyl D

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take the bark of Elephus chinensis and crush it through 40 meshes, take 1kg of raw materials and add supercritical CO 2 In the extraction kettle, turn on the equipment and adjust the equipment parameters: the extraction temperature is 55°C, the extraction pressure is 30MPa, the temperature of the separation kettle I is 45°C, the pressure is 9MPa, the temperature of the separation kettle II is 35°C, the pressure is 7MPa, and CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 20 L / h, and 1.2 L of 95% ethanol aqueous solution was added, and the dynamic extraction was performed for 4 hours. The extract was collected, ethanol was recovered, and heptane was added to degrease to obtain a crude extract. Take n-hexane, ethyl acetate, methanol, and water, mix them in a ratio of 1:5:3:3, 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 850rpm,...

Embodiment 2

[0016] Take the bark of Elephus chinensis and crush it through 40 meshes, take 1kg of raw materials and add supercritical CO 2 In the extraction kettle, turn on the equipment and adjust the equipment parameters: the extraction temperature is 42°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, the pressure is 6.5MPa, and CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 18L / h, and 1.8L of 95% ethanol aqueous solution was entrained, and the dynamic extraction was performed for 3 hours. The extract was collected, the ethanol was recovered, and heptane was added to degrease to obtain a crude extract. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 3:6:4:4. Take the upper phase and pump it into the separation column until the separation column is filled with the stationary phase at a spe...

Embodiment 3

[0018] Take the bark of Elephus chinensis and crush it through 40 meshes, take 1kg of raw materials and add supercritical CO 2 In the extraction kettle, turn on the equipment and adjust the equipment parameters: the extraction temperature is 45°C, the extraction pressure is 25MPa, the temperature of the separation kettle I is 35°C, the pressure is 8MPa, the temperature of the separation kettle II is 28°C, the pressure is 6MPa, and CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 19L / h, and 2L of 95% ethanol aqueous solution was entrained, and the dynamic extraction was performed for 2 hours. The extract was collected, ethanol was recovered, and heptane was added to degrease to obtain a crude extract. Take n-hexane, ethyl acetate, methanol, and water, mix them in a ratio of 2:4:2:3, 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...

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PUM

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Abstract

The invention belongs to the field of natural drug chemistry, and relates to a method for preparing Wikstroelide D. The method comprises the following steps: pulverizing Wikstroemia retusa A.Gray bark while controlling the particle size at 40-80 meshes, adding into an extraction kettle, carrying out CO2 extraction by using a 90-100 vol% ethanol water solution as an entrainer, collecting the extract, recovering the ethanol, degreasing with heptane, carrying out high-speed counter-current chromatography separation by using n-hexane-ethyl acetate-methanol-water as a solvent system, and drying the fraction under reduced pressure to obtain the Wikstroelide D. The Wikstroelide D product prepared by the method provided by the invention has the advantages of no pollution and high yield; and the method is suitable for industrialized preparation of Wikstroelide D.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a method using supercritical CO 2 Extraction and high-speed counter-current chromatographic separation techniques for the preparation of annelid D. Background technique [0002] Wikstroelide D (Wikstroelide D) is a diterpenoid compound with molecular formula C 52 h 80 o 11 , molecular weight 881.2. Elephant D is widely found in natural plants, mainly from the spice plant Elephant indentatus Wikstroemia retusa A.Gray isolated from the bark. Pharmacological studies have shown that catkin D has cytotoxic activity, and in the MTT test, it has cytotoxic activity to P388 and human lung cancer strain PC-6. [0003] At present, there is no domestic report on the method of preparing a large amount of anthelin D. Contents of the invention [0004] The object of the present invention is to provide a kind of method for preparing keloid D. [0005] In order to achieve the ...

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