Method for supercritical fluid extraction of amentoflavone

A technology of double flavone and supercritical fluid is applied in bulk chemical production, organic chemistry and other directions, can solve the problems of low extraction rate, large amount of organic solvent, complicated steps, etc., and achieves low extraction temperature, short production cycle, good separation effect

Inactive Publication Date: 2011-09-14
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, traditional separation methods such as macroporous resin adsorption, silica gel column chromatography, Sephadex LH-20, etc. are mainly used for the separation of am...

Method used

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  • Method for supercritical fluid extraction of amentoflavone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The dried Selaginella is crushed into a coarse powder, and 2 kg is put into an extraction kettle for supercritical CO 2 Fluid extraction. Extraction conditions: Heat the extraction tank to 37°C, and the analysis tanks I and II to 20°C through a heat exchanger. CO cooling by refrigeration equipment 2 storage tank, open CO 2 Steel cylinder, the flow rate is 30L / h, turn on the booster pump to increase the pressure of the extraction kettle to 23MPa, and the pressure of the analysis kettle Ⅰ and Ⅱ to 6MPa, turn off the CO 2 Cylinder valve. Open the cycle, add 100ml of acetone carrier to the carrier storage tank, and then open the valve of the carrier high-pressure pump to pump the carrier into the extraction kettle. After 3 hours of extraction, open the outlets of the analysis kettle Ⅰ and Ⅱ to collect the released extraction things. The extract was dissolved by heating under reflux with 60% ethanol, added polyamide, stirred evenly, dried at low temperature, added to a ...

Embodiment 2

[0021] The dried Selaginella is crushed into a coarse powder, and 2 kg is put into an extraction kettle for supercritical CO 2 Fluid extraction. Extraction conditions: Heat the extraction tank to 45°C, and the analysis tanks I and II to 33°C through a heat exchanger. CO cooling by refrigeration equipment 2 storage tank, open CO 2 Steel cylinder, the flow rate is 26L / h, turn on the booster pump to increase the pressure of the extraction kettle to 33MPa, and the analysis kettle I and II to 8MPa, turn off the CO 2 Cylinder valve. Open the cycle, add 400ml of ethanol carrier to the carrier storage tank, then open the valve of the high-pressure pump of the carrier to pump the carrier into the extraction kettle. After 5 hours of extraction, open the outlets of the analysis kettle Ⅰ and Ⅱ to collect the released extraction thing. The extract was dissolved by heating under reflux with 60% ethanol, added polyamide, stirred evenly, dried at low temperature, added to a pretreated po...

Embodiment 3

[0023] The dry Selaginella is crushed into a coarse powder, and 5 kg is put into an extraction kettle for supercritical CO 2 Fluid extraction. Extraction conditions: heat the extraction tank to 50°C, and the analysis tanks I and II to 40°C through a heat exchanger. CO cooling by refrigeration equipment 2 storage tank, open CO 2 The steel cylinder, the flow rate is 22L / h, turn on the booster pump to increase the pressure of the extraction kettle to 38MPa, and the analysis kettle Ⅰ and Ⅱ to 9MPa, turn off the CO 2 Cylinder valve. Open the cycle, add 1250ml of acetone carrier to the carrier storage tank, and then open the valve of the carrier high-pressure pump to pump the carrier into the extraction kettle. After 4 hours of extraction, open the outlets of the analysis kettle Ⅰ and Ⅱ to collect the released extraction things. The extract was dissolved by heating under reflux with 60% ethanol, added polyamide, stirred evenly, dried at low temperature, added to a pretreated po...

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Abstract

The invention relates to a method for supercritical fluid extraction of amentoflavone. In the method, a supercritical CO2 extraction-column chromatography-recrystallization combination technology is adopted to prepare high-purity amentoflavone; the conditions of the supercritical CO2 extraction are as follows: ethanol or acetone is used as an entrainer, the flow of CO2 is 22-35L/h, the pressure of an extraction kettle is 23-38MPa, the temperature of the extraction kettle is 35-50 DEG C, and extraction time is 3-6 hours. The method specifically comprises the following steps: carrying out supercritical extraction with the parameters; analyzing so as to obtain extractive; separating and purifying the extractive through polyamide column chromatography; eluting with chloroform-acetone-methanol; and recrystallizing with an ethanol aqueous solution so as to obtain the finished product. The separation method is simple and is easy to apply in industrial production, and the product is pure.

Description

Technical field: [0001] The invention belongs to the technical field of separation of effective components of traditional Chinese medicines, and in particular relates to a method for extracting amiflavonoids from Pine japonica with a supercritical fluid. Background technique: [0002] Selaginella, also known as Nine Dead Resurrection Grass, is the dry whole grass of Selaginella tamariscina (Beauv.) Spring or Selaginella pulvinata (Hook.et Grev.) Maxim. In my country, it is mainly distributed in Guangdong, Guangxi, Fujian, Taiwan, Zhejiang, Jiangsu, Jiangxi, Hunan and other places. It can be collected in spring and autumn, and the source of medicine is rich. Selaginella has the functions of clearing heat and detoxifying, promoting blood circulation and removing blood stasis, hemostasis and anti-cancer, anti-cancer, anti-cancer, anti-inflammation, anti-virus, anti-infection, anti-allergic, analgesic, hypnotic, lowering blood pressure, lowering blood sugar, and enhancing human...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
CPCY02P20/54
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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