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Method for extracting juglone from walnut green husk residue by microwave reflux

A technology of microwave reflux and walnut green husk, which is applied in quinone separation/purification, organic chemistry, etc., to achieve the effects of avoiding thermal decomposition, high extraction rate and wide application

Inactive Publication Date: 2010-12-08
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the use of microwave reflux to extract and purify natural products such as medicines and foods is attracting widespread attention. However, after searching, there is no report on the method of extracting juglone from walnut green peel waste residue with chloroform as a solvent.

Method used

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  • Method for extracting juglone from walnut green husk residue by microwave reflux

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 10 kg green bark is crushed with a crusher and filtered. Take the crushed material and adjust the solid-liquid ratio to 1:8 with chloroform, put it in a microwave oven reflux device, and extract it under a microwave power series for 25 minutes under a warm fire, remove it and filter it with suction to obtain a juglone quinone leaching solution. Extract the filter residue once more, wash the filter residue with solvent for 3 times, collect all the solution, and concentrate by rotary evaporation under reduced pressure to obtain the product juglone. Chloroform is recycled.

[0021] The product juglone was tested for each index. Wherein, by AVATAR360 type Fourier transform infrared spectrometer, obtain juglone standard substance and sample collection of illustrative plates (see attached figure 1 ), and analyzed and compared, it was determined that the product was juglone.

[0022] The calculated juglone extraction rate was 85%, the purity was 92%, and the yield was 0.19%...

Embodiment 2

[0028] 10 kg green bark is crushed with a crusher and filtered. Take the crushed material and adjust the solid-liquid ratio to 1:5 with chloroform, put it in a microwave oven reflux device, and extract it under a microwave power series for 30 minutes under a warm fire, remove it and filter it with suction to obtain a juglone extract. Extract the filter residue once more, combine the two extracts, wash the filter residue 5 times with a solvent, collect all the solutions, and concentrate by rotary evaporation under reduced pressure to obtain the product juglone. Chloroform is recycled. The product juglone was tested for each index. The extraction rate of juglone was 93%, the purity was 81.5%, and the yield was 0.20%.

Embodiment 3

[0030] 10 kg green bark is crushed with a crusher and filtered. Take the crushed material and adjust the solid-liquid ratio to 1:6 with chloroform, put it in a microwave oven reflux device, and extract it under a microwave power series for 20 minutes under a warm fire, remove it and filter it with suction to obtain a juglone quinone leaching solution. Extract the filter residue once more, combine the two extracts, wash the filter residue 4 times with a solvent, collect all the solutions, and concentrate by rotary evaporation under reduced pressure to obtain the product juglone. Chloroform is recycled. The product juglone was tested for each index. The extraction rate of juglone was 88%, the purity was 85%, and the yield was 0.19%.

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Abstract

The invention discloses a method for extracting juglone from walnut green husk residue by microwave reflux, which ueses chloroform solvent for extraction by a microwave reflux extraction method, preferably adopting walnut epicarpe (green husk) residue with higher juglone content and can be obtained easily as raw materials for extraction. The method is carried out under the optimal extraction condition that the solid-to-liquid ratio of walnut green husk with average grain size of 50 mesh to the chloroform solvent is between 1:5 and 1:8, and comprises the steps of: subjecting walnut green husk residue to extraction and pumping filtration at soft fire in microwave power level and washing the filter residue with solvent to obtain juglone extraction liquid, collecting all solutions, and preparing the juglone by decompression, rotary evaporation and concentration. After all index measurements, the extraction ratio of the juglone is 92%, the purity of product is 81.5%, and the product yield is 0.20%. The method is rapid and convenient, and has high extraction ratio, and devices in the method are easy to operate, have low energy consumption, consume less solvents which are easy to be recovered, and are suitable for the expanded production in factories. Meanwhile, the problem that juglone is heated and decomposed in a traditional method can be effectively avoided, which guarantees the effectiveness of extractives. The method satisfies the environmental protection and industrialization demands. The extracted juglone can be widely applied, and active ingredients in the juglone have the effects of antibacterial, anticancer and sedation of central nervous system, and have wide application prospects in such fields as medicine, pesticide, dye, pH indicator and the like.

Description

technical field [0001] The invention relates to a method for extracting juglone, more particularly, to a microwave reflux extraction method for natural active ingredient juglone. Background technique [0002] Juglone is an active ingredient extracted from the immature exocarp (green skin) of the Juglandaceae plant - Juglans and its congener black walnut. It has antibacterial, anticancer and central nervous system sedative effects. The juglone precipitated from the mixture of benzene and petroleum ether is orange-yellow needle crystal, and the juglone precipitated from chloroform is red-yellow prismatic crystal, which has a special odor and has a melting point of 155°C and can be sublimated; and With water vapor can be volatile. Juglone is insoluble in cold water, slightly soluble in hot water, soluble in ethanol and ether, and miscible with chloroform and benzene. When it is dissolved in alkali solution, it is purple red, and when it is dissolved in concentrated sulfuric a...

Claims

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Application Information

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IPC IPC(8): C07C50/32C07C46/10
Inventor 刘淑萍闫路省李秀凤
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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