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Method for extracting (20R)-22E-24-ethyl cholane-4,22-diene-3-ketone from stems and leaves of Coix lacryma-jobi

A technology of ethylcholestane, -22E-24-, applied in the field of extracting -22E-24-ethylcholestane-4,22-dien-3-one, which can solve resource waste, coix stems and leaves Insufficient utilization and other problems, to achieve the effect of prolonging the service life, good economic and ecological benefits, and improving utilization

Inactive Publication Date: 2017-11-24
右江民族医学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The stems and leaves of Coix coix have not been fully utilized, and most of them are discarded as waste, resulting in a great waste of resources

Method used

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  • Method for extracting (20R)-22E-24-ethyl cholane-4,22-diene-3-ketone from stems and leaves of Coix lacryma-jobi
  • Method for extracting (20R)-22E-24-ethyl cholane-4,22-diene-3-ketone from stems and leaves of Coix lacryma-jobi
  • Method for extracting (20R)-22E-24-ethyl cholane-4,22-diene-3-ketone from stems and leaves of Coix lacryma-jobi

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Experimental program
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Effect test

Embodiment 1

[0033] A method for extracting (20R)-22E-24-ethylcholestane-4,22-dien-3-one from coix stems and leaves, comprising the following steps:

[0034] (1) Alcohol extraction: crush the dried Coix coix stems and leaves, add 8 times the weight of 90% ethanol, heat to 60°C, reflux extraction for 3 times, each time for 2.5h, combine the extracts, concentrate under reduced pressure to obtain the extract A ;

[0035] (2) Extraction: disperse the extract A of step (1) with water, extract 3 times with 8 times the weight of petroleum ether, combine the extracted parts of petroleum ether, and concentrate to obtain extract B;

[0036] (3) primary column chromatography: the extract B of step (2) is chromatographed on a 200-300 mesh silica gel column, and is eluted with a gradient of sherwood oil-ethyl acetate with a volume ratio of 15:1 to 5:1. The eluate was detected by TLC, and the eluate containing (20R)-22E-24-ethylcholestane-4,22-dien-3-one was collected;

[0037] (4) Secondary column ch...

Embodiment 2

[0041] A method for extracting (20R)-22E-24-ethylcholestane-4,22-dien-3-one from coix stems and leaves, comprising the following steps:

[0042] (1) Alcohol extraction: crush the dried Coix coix stems and leaves, add 12 times the weight of 90% ethanol, heat to 70°C, reflux extraction 5 times, each time for 1.5h, combine the extracts, concentrate under reduced pressure to obtain the extract A ;

[0043] (2) Extraction: disperse the extract A of step (1) with water, extract 5 times with 12 times the weight of petroleum ether, combine the extracted parts of petroleum ether, and concentrate to obtain extract B;

[0044] (3) primary column chromatography: the extract B of step (2) is chromatographed on a 200-300 mesh silica gel column, and is eluted with a gradient of sherwood oil-ethyl acetate with a volume ratio of 15:1 to 5:1. The eluate was detected by TLC, and the eluate containing (20R)-22E-24-ethylcholestane-4,22-dien-3-one was collected;

[0045](4) Secondary column chrom...

Embodiment 3

[0049] A method for extracting (20R)-22E-24-ethylcholestane-4,22-dien-3-one from coix stems and leaves, comprising the following steps:

[0050] (1) Alcohol extraction: crush the dried Coix coix stems and leaves, add 8-12 times the weight of 90% ethanol, heat to 65°C, reflux extraction 4 times, 2 hours each time, combine the extracts, concentrate under reduced pressure to obtain the extract A;

[0051] (2) Extraction: disperse the extract A of step (1) with water, extract 4 times with 10 times the weight of petroleum ether, combine the extracted parts of petroleum ether, and concentrate to obtain extract B;

[0052] (3) primary column chromatography: the extract B of step (2) is chromatographed on a 200-300 mesh silica gel column, and is eluted with a gradient of sherwood oil-ethyl acetate with a volume ratio of 15:1 to 5:1. The eluate was detected by TLC, and the eluate containing (20R)-22E-24-ethylcholestane-4,22-dien-3-one was collected;

[0053] (4) Secondary column chro...

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Abstract

The invention discloses a method for extracting (20R)-22E-24-ethyl cholane-4,22-diene-3-ketone from stems and leaves of Coix lacryma-jobi. The method comprises the following steps: dried stems and leaves of Coix lacryma-jobi are crushed, ethanol is added and heated, reflux extraction is carried out, and an extracting solution is condensed in order to obtain an extract A; water is added into the extract A and the extract A is dispersed, petroleum ether is used for extraction, and petroleum ether is partially condensed in order to obtain an extract B; silica gel column chromatography is carried out for the extract B firstly, petroleum ether-ethyl acetate gradient elution is carried out, separated and purified components are collected, chromatography is carried out, pure dichloromethane is used for elution, separated and purified components are separated and purified by preparation type high performance liquid chromatography, a tR=31 min component is collected, condensation and crystallization are carried out, and the product is obtained. (20R)-22E-24-ethyl cholane-4,22-diene-3-ketone is extracted from waste stems and leaves of Coix lachrymal-jobi, environmental pollution is reduced, utilization rate of stems and leaves of Coix lacryma-jobi is improved, an industry chain of Coix lacryma-jobi is prolonged, income of Coix lacryma-jobi industry is increased, and the method has good economic benefits and ecological benefits.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for extracting (20R)-22E-24-ethylcholestane-4,22-dien-3-one from coix coix stems and leaves. Background technique [0002] Coix lachryma-jobi L. belongs to the Gramineae genus Coix. It is sweet and light in taste and slightly cold in nature. It has the effects of invigorating the spleen, nourishing the lungs, clearing away heat and dampness, and is known as the "king of nourishment and health care". . Coix is ​​a treasure for the whole body. Coix stems can prevent and treat measles and eczema. The alkaloids contained in Coix leaves have the functions of clearing away heat and dampness, invigorating the spleen and killing insects, warming the stomach and nourishing qi, soothing the pan and promoting blood circulation. The medicinal parts such as the roots, stems and leaves, and seeds of Coix coix are widely used in 15 ethnic groups including Zhuang, Mongolian...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 黄锁义喻巧容李庭树林瑶
Owner 右江民族医学院
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