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Method for extracting isofraxidin

A technology of isoquinpin and an extraction method, which is applied in the field of biological enzymolysis and recrystallization to extract isoquinpin, can solve the problems of severe reaction, low extraction yield and poor reproducibility in the operation process, and achieves easy industrialization and high yield. , process mild effect

Inactive Publication Date: 2011-02-09
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] As mentioned above, the existing technology has the problems of low extraction yield, severe reaction in the operation process, small production volume and poor reproducibility.

Method used

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  • Method for extracting isofraxidin

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Acanthopanax senticosus is removed and crushed to 40 meshes, take 1kg, add 200ml of water, mix well and add 5g of cellulase, natural enzymatic hydrolysis for 5 days, take it out and add 6L80% methanol to reflux extraction for 1 hour to extract 3 times, the extract is rotated The evaporator recovers methanol, adds 4BV ethyl acetate to the concentrated solution, heats to dissolve and remove the water layer, adds activated carbon alumina (1:4) column for decolorization, collects the injection liquid and recovers ethyl acetate under reduced pressure to 1 / 8 of the original volume, and adds a small amount of Stir with petroleum ether until precipitation occurs, and place to crystallize; filter out the crude crystals, reflux with chloroform and acetone in turn, dissolve and refrigerate, refrigerate to crystallize at 0-4°C, and dry under vacuum and low pressure to obtain 3.4 g of isoferidin, with a content of 95%.

Embodiment 2

[0033] Acanthopanax senticosus is removed and crushed to 80 mesh, take 5kg, add 800ml of water, mix well and add 5g of β-glucanase, natural enzymolysis for 10 days, take it out and put it into a multi-functional extraction tank, add 50L of 90% methanol for reflux extraction for 2 hours to extract 2 Once, combine the extracts to recover methanol, add 9BV ethyl acetate to the concentrated solution, heat to dissolve and remove the water layer, add activated carbon alumina (1:6) column for decolorization, collect the injection solution and recover ethyl acetate under reduced pressure to 1 / 3 of the original volume , add a small amount of petroleum ether and stir until precipitation occurs, leave to crystallize; filter out the crude crystals, reflux with chloroform and acetone in turn, dissolve and refrigerate, and refrigerate to crystallize at 0-4°C, dry under vacuum and low pressure to obtain 20 g of isoferidin, with a content of 98%.

Embodiment 3

[0035] Acanthopanax senticosus is removed and crushed to 60 mesh, take 5kg, add 1000ml of water, mix well and then add 15g of naringinase, natural enzymolysis for 7 days, take it out and put it into a multi-functional extraction tank, add 75L85% methanol for reflux extraction for 3 hours for extraction once, Combine the extracts to recover methanol, add 6BV ethyl acetate to the concentrated solution, heat to dissolve and remove the water layer, add activated carbon alumina (1:3) column for decolorization, collect the injection solution and recover ethyl acetate under reduced pressure to 1 / 5 of the original volume, add Stir with a small amount of petroleum ether until precipitation occurs, and place to crystallize; filter out the crude crystals, reflux with chloroform and acetone in turn to dissolve and refrigerate, refrigerate to crystallize at 0-4°C, and dry under vacuum and low pressure to obtain 14 g of isoferidin, with a content of 97%.

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Abstract

The invention relates to a method for extracting isofraxidin, which comprises the following steps of: pulverizing acanthopanax root serving as a raw material, and adding 10 to 20 percent water for wetting; adding biological enzyme for enzymolysis in the normal state for 3 to 10 days, and after the enzymolysis, extracting through the reflux in 80 to 90 percent methyl alcohol; and concentrating extracting solution under reduced pressure, adding ethyl acetate for dissolving to remove aqueous layer, decolorizing through an activated carbon alumina mixed column to remove impurities, concentrating and crystallizing, recrystallizing through the reflux of chloroform and acetone, and drying crystals at the low temperature to obtain the isofraxidin. In the method for extracting the isofraxidin, the product yield is high, the operation is simple, the repeatability is good, and the enlargement production is easy to perform.

Description

Technical field: [0001] The invention relates to a method for extracting isoferdine, in particular to a method for extracting isoferdine through biological enzymolysis and recrystallization. Background technique: [0002] Isoferdine is also called isoferidin, isoferdine, and coumarin compounds. [0003] Molecular formula: C 11 h 10 o 5 [0004] Molecular structural formula:: [0005] [0006] Isoferidin Eleutheroside B 1 [0007] Soluble in methanol, ethanol, acetone, chloroform, boiling water, alkaline aqueous solution, slightly soluble in ether, hardly soluble in petroleum ether and cold water. Isoferdinine has calming and sedative effects, can shorten the time to fall asleep, improve sleep quality, and has anti-inflammatory and anti-tumor effects. [0008] The content of free isoferdinine in Acanthopanax senticosus is not high, only about 0.3%, and part of it is isoferdinine in compound state, that is, eleutheroside. The hydrolysis of arginica glycosides. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/18C12P17/06
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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