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Method for extracting vernodalin from vernonia anthelmintica

A technology for repelling Vernonia and Vernonia, applied in the field of natural medicinal chemistry, can solve the problems of sample loss, poor reproducibility, and difficulty in realization, and achieve the effects of short preparation cycle, overcoming sample dead adsorption, and low energy consumption.

Inactive Publication Date: 2012-01-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Silica gel column chromatography has technical defects such as serious sample loss and poor reproducibility, which is difficult to realize in the industrial production of vernonia

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The insect-repelling Vernonia medicinal material is crushed into 80 meshes, and 1000g of the raw material is added to supercritical CO 2 In the extraction kettle, turn on the equipment and set the parameters: the extraction temperature is 60°C, the extraction pressure is 23MPa, the temperature of the separation kettle I is 60°C, the pressure is 9MPa, the temperature of the separation kettle II is 45°C, and the pressure is 5MPa. into CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 20L / h, and anhydrous methanol was entrained at 300ml / h. Dynamic extraction was performed for 3 hours. The extract was collected, methanol was recovered, and washed with petroleum ether for 3 times to obtain 25g of extract. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 4:7:5:5. Take the upper phase and inject it into the chromatographic tube as the stationary phase. Turn on the high-speed countercurrent chroma...

Embodiment 2

[0017] The insect repelling Vernonia medicinal material is crushed into 20 meshes, and 1000g of the raw material is added to supercritical CO 2 In the extraction kettle, turn on the equipment and set the parameters: the extraction temperature is 65°C, the extraction pressure is 18MPa, the temperature of the separation kettle I is 50°C, and the pressure is 7MPa, the temperature of the separation kettle II is 50°C, and the pressure is 6MPa. into CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 25L / h, and entrained with anhydrous methanol 400ml / h, and extracted dynamically for 2h, the extract was collected, methanol was recovered, and washed twice with petroleum ether to obtain 22g of extract. Take n-hexane, ethyl acetate, methanol, and water, mix them in a ratio of 4:6:5:5, take the upper phase and inject it into the chromatographic tube as the stationary phase, turn on the high-speed countercurrent chromatograph, adjust the ...

Embodiment 3

[0020] The insect-repelling Vernonia medicinal material is crushed into 60 meshes, and 1000g of the raw material is added to supercritical CO 2 In the extraction kettle, turn on the equipment and set the parameters: the extraction temperature is 60°C, the extraction pressure is 20MPa, the temperature of the separation kettle I is 60°C, the pressure is 8MPa, the temperature of the separation kettle II is 45°C, and the pressure is 5MPa. into CO 2 Fluid, after reaching the above parameters, with CO 2 The liquid was extracted at a flow rate of 22L / h, and anhydrous methanol was entrained at 400ml / h. Dynamic extraction was performed for 3 hours. The extract was collected, methanol was recovered, and washed with petroleum ether for 3 times to obtain 26g of extract. Take n-hexane, ethyl acetate, methanol, and water, mix them in a ratio of 4:7:6:5, take the upper phase and inject it into the chromatographic tube as the stationary phase, turn on the high-speed countercurrent chromatogr...

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PUM

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Abstract

The invention belongs to the chemical field of natural medicines, and discloses a method for extracting vernodalin from vernonia anthelmintica. The method comprises the steps of: by taking vernonia anthelmintica as a raw material, crushing and sieving with sieves of 20-80 meshes; adding the vernonia anthelmintica in an extraction kettle, and collecting an extract liquid by taking absolute methanol as an entrainer and adopting supercritical CO2 extraction; recovering methanol to obtain extracts; degreasing through petroleum ether; then separating the extracts by taking n-hexane-ethyl acetate-methanol-water as a solvent system and adopting a high-speed countercurrent chromatography; and depressurizing and concentrating an eluate to obtain vernodalin. The method disclosed by the invention adopts the supercritical CO2 extraction and a high-speed countercurrent chromatographic separation technology, and is highly efficient, environment-friendly and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a method for extracting vernonia macropicrin from insect-repelling vernonia. Background technique [0002] Vernodalin is a sesquiterpene compound, chemical name 2-Propenoic acid, 2-(hydroxymethyl)-, 5a-ethenyldecahy-dro-3,9-bis(methylene)-2, 8-dioxo-2H -furo[2,3-f]benzopyran-4ylester, [3aR-(3aα, 4aα, 5aα, 9aα, 9bβ)-, molecular formula C19H20O7, molecular weight 360.35. High-purity Vernonia macropicrin is a colorless oil, (α)24D+125°(C=1.35, chloroform), soluble in methanol, ethanol, acetone, etc., insoluble in water, petroleum ether, etc. Vernonia macrocin has antibacterial, insecticidal, antimalarial, and antitumor activities. [0003] Insect-repelling Vernonia is the fruit of the insect-repelling Vernonia dicotyledonous plant Asteraceae. Insect-repelling Vernonia was first recorded in "Flora of China". The fruit is bitter in taste and cool in nature...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
CPCY02P20/54
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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