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Method for preparing Amorfrutin A and Amorfrutin B from amorpha fruticosa fruits

An amorpha and fruit technology, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of unsuitability for industrial production, complex process, many by-products, etc., and achieves short cycle, simple process and low cost. Effect

Active Publication Date: 2019-01-01
陕西嘉禾药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to solve the disadvantages of existing preparation methods such as complex process, long period, low yield, many by-products, and being unsuitable for industrialized production, and provides a method for preparing Amorfrutin A and Amorfrutin B from the fruit of Amorpha fruticosa method

Method used

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  • Method for preparing Amorfrutin A and Amorfrutin B from amorpha fruticosa fruits
  • Method for preparing Amorfrutin A and Amorfrutin B from amorpha fruticosa fruits

Examples

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Embodiment 1

[0044] A method for preparing Amorfrutin A and Amorfrutin B from amorpha fruit, comprising the following steps:

[0045] Step 1) subcritical extraction

[0046] Take 100Kg of Amorpha fruticosa fruit and crush it, pass it through a sieve of 80 mesh to 100 mesh, add 0.5 times the mass of cyclohexane and mix well, leave it at room temperature for more than 1 hour, then put it into the extraction kettle, the extraction pressure is 15MPa, and the extraction temperature is 30°C Under subcritical extraction for 2 hours, an oily extract was obtained;

[0047] Step 2) Remove impurities

[0048]Add 5 times its mass to the oily extract obtained in step 1), and add an ethylenediamine solution with a mass concentration of 10%, stir to dissolve, and collect the ethylenediamine solution layer, then add hydrochloric acid solution to the ethylenediamine solution layer Adjust the pH to 3-5, let stand, perform the first filtration, collect the precipitate and wash the precipitate to neutrality...

Embodiment 2

[0057] A method for preparing Amorfrutin A and Amorfrutin B from amorpha fruit, comprising the following steps:

[0058] Step 1) subcritical extraction

[0059] Take 100Kg of Amorpha fruticosa fruit and grind it through a 80-mesh to 100-mesh sieve, add acetone equal to its mass and mix well, place it at room temperature for more than 1 hour, and then put it into an extraction kettle with an extraction pressure of 25MPa and an extraction temperature of 50°C for sub- Critical extraction for 5 hours to obtain an oily extract;

[0060] Step 2) Remove impurities

[0061] In the oily extract that step 1) obtains, add its quality 15 times amount, the DMF solution that mass concentration is 20%, stir and dissolve, and collect DMF solution layer, then add citric acid solution in DMF solution layer and adjust pH to 3 ~ 5. Stand still, perform the first filtration, collect the precipitate and wash the precipitate with water until neutral;

[0062] Step 3) mixed solvent separation

[...

Embodiment 3

[0070] A method for preparing Amorfrutin A and Amorfrutin B from amorpha fruit, comprising the following steps:

[0071] Step 1) subcritical extraction

[0072] Take 100Kg of Amorpha fructus fruit and crush it, pass it through a sieve of 80-100 mesh, add 0.9 times its mass of dichloromethane and mix well, leave it at room temperature for more than 1 hour, then put it into the extraction kettle, the extraction pressure is 20MPa, and the extraction temperature is 40°C Under subcritical extraction for 3 hours, an oily extract was obtained;

[0073] Step 2) Remove impurities

[0074] To the oily extract obtained in step 1), add a triethylamine solution with 7 times its mass and a mass concentration of 15%, stir to dissolve, and collect the triethylamine solution layer, then add glacial acetic acid to the triethylamine solution layer Adjust the pH of the solution to 3-5, let it stand still, perform the first filtration, collect the precipitate and wash the precipitate to neutrali...

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Abstract

The invention provides a method for preparing Amorfrutin A and Amorfrutin B from amorpha fruticosa fruits, which solves the defects of such as complex process, long period, low yield, excessive byproduct and unsuitability for industrial production of existing preparation method. The method comprises four steps, i.e. subcritical extraction, impurity removal, mixed solvent separation and purification. Firstly, by utilizing the low polarity characteristic of Amorfrutin A and Amorfrutin B, organic solvent is adopted to separate the Amorfrutin A and the Amorfrutin B out from the material by the method of wetting the amorpha fruticosa fruits before extraction; secondly, by utilizing the acidic characteristic of the Amorfrutin A and te Amorfrutin B, an alkaline organic solvent is utilized to dissolve the Amorfrutin A and the Amorfrutin B to remove most of impurities, and an acidic solution is utilized to acidify the alkaline solution, so that the Amorfrutin A and the Amorfrutin Bare separated out; thirdly, by utilizing the characteristic of different polarities of the Amorfrutin A and the Amorfrutin B, mixed reagent is utilized to separate the Amorfrutin A and the Amorfrutin B; and finally, methods, such as refrigerated centrifugation and rinsing, are utilized to further remove low-polarity impurities, so that the Amorfrutin A and the Amorfrutin B are respectively purified.

Description

technical field [0001] The invention belongs to the field of natural product extraction technology, in particular to a method for preparing Amorfrutin A and Amorfrutin B from the fruit of Amorpha fruticosa. Background technique [0002] Amorpha fruticosa Linn. is a deciduous shrub of the genus Amorpha fruticosa. It is native to the northeastern and southeastern United States. It is an excellent soil and water conservation and nectar source plant; it is now in Northeast China, North China, Northwest China and Shandong , Anhui, Jiangsu, Henan, Hubei, Guangxi, Sichuan and other provinces and regions are all cultivated; it has the effect of dispelling dampness and reducing swelling, and is mainly used to treat carbuncles, eczema, burns and scalds. [0003] The fruit of Amorpha fruticosa is rich in lipid components, in addition to rich in Amorfrutin, Amorfrutin can well control and activate the selective expression of nuclear receptor PPARγ (an important receptor for sugar and li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C65/28
CPCC07C51/42C07C65/28
Inventor 张瑜肖红耿道元王晓莹
Owner 陕西嘉禾药业有限公司
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