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Method for extracting fraxinellone through subcritical fluid

A subcritical fluid and a technology for extracting alkone, which is applied in the biological field, can solve the problems of large amount of organic reagents, high equipment cost, and high energy consumption, and achieve the effects of high extraction efficiency, less solvent consumption, and simple purification steps

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

[0006] The preparation methods of alkone mostly use conventional organic reagent extraction and supercritical CO 2 Patent (200810017515.7) "New application of alkone and alkone aqueous insecticide" adopts petroleum ether reflux extraction, methanol-petroleum ether mixed solvent is added to precipitate crude crystals, and then purified by column chromatography. High energy consumption and large amount of organic reagents
Another example (Application No.: 201010510886.6) "A method for extracting alkone from white fresh bark", this patent uses supercritical CO2 extraction, which is an efficient and clean method, but the equipment is expensive and difficult to industrialize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dry and pulverize the white fresh skin, take 1Kg, put it into a subcritical extraction kettle, pass through 5L of 80% ethanol solution, and extract dynamically for 40min at a temperature of 110°C and a pressure of 0.4 Mpa, extract the reagent under reduced pressure, and add the concentrated solution Adsorbed in D101 macroporous resin, eluted with 5 times the column volume of 70% ethanol solution, concentrated the eluent, extracted the concentrated solution with petroleum ether for 3 times, collected the petroleum ether layer to recover the reagent, and obtained 1.4 g of white alkone powder.

Embodiment 2

[0022] Dry and pulverize the white fresh skin, take 1Kg, put it into a subcritical extraction kettle, pass through 6L of 70% methanol solution, and extract dynamically for 50min at a temperature of 120°C and a pressure of 0.8 Mpa, extract the reagent under reduced pressure, and add the concentrated solution Adsorbed in AB-8 macroporous resin, eluted with 4 times the column volume of 80% ethanol solution, concentrated the eluent, extracted the concentrate twice with petroleum ether, collected the petroleum ether layer to recover the reagent, and obtained 1.7 g of white alkone powder.

Embodiment 3

[0024] Dry and pulverize the white fresh skin, take 1Kg, put it into a subcritical extraction kettle, pass through 5L of 70% acetone solution, and extract dynamically for 60min at a temperature of 90°C and a pressure of 0.5 Mpa, extract the reagent under reduced pressure, and add the concentrated solution Adsorbed in HZ-816 macroporous resin, eluted with 4 times column volume of 90% ethanol solution, concentrated eluent, extracted 3 times with petroleum ether, collected petroleum ether layer to recover reagent, and obtained 1.6 g of white alkone powder.

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Abstract

The invention discloses a method for extracting fraxinellone through subcritical fluid. The method comprises the steps as follows: drying and crushing cortex dictamni, and adding to a subcritical extracting kettle; adding a polar organic solvent, and dynamically extracting for 30 to 80 minutes at 80 to 120 DEG C under pressure of 0.2 to 1Mpa to obtain extract; recovering reagent under reduced pressure to obtain concentrated solution; adding the concentrated solution to macroporous resin to be absorbed; eluting with 4 to 7 times of 60-90% ethanol solution based on column volume; concentrating eluant; extracting the concentrated eluant with petroleum ether for two to three times; collecting the petroleum ether layer, and recovering the reagent to obtain fraxinellone. With the adoption of the method for extracting fraxinellone disclosed by the invention, little solvent is used, energy comsumption is low, high efficiency is ensured, and industrial operation is easy to carry out.

Description

technical field [0001] The invention belongs to the field of biotechnology, in particular to a method for extracting arketone with a subcritical fluid. Background technique [0002] Radix Radix Cortex is Rutaceae Radix Radix Radix ( Dictamnus dasycarpus Turcz ) dry root bark has the effects of expelling wind, dampness, clearing away heat, detoxification, etc. Studies in recent years have shown that alkone is the main medicinal ingredient of Cortex Dictatus, which has good liver protection, enzyme reduction and liver fibrosis inhibition activities, and has antibacterial and insecticidal activities. It has been used as a new type of liver disease. medicine. [0003] Ashone is a white needle-like crystal with a melting point of 116~117°C, easily soluble in ethanol, ethyl acetate, petroleum ether and other organic reagents, but hardly soluble in water. Molecular formula: C 14 h 16 o 3 , molecular weight: 232.28, [0004] Structural formula: [0005] . [0006] The pre...

Claims

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Application Information

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IPC IPC(8): C07D307/88
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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