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Method for extracting and refining ecdysterone

A technology of ecdysterone and extract solution, which is applied in the field of natural compound extraction, can solve the problems of high concentration temperature, long concentration time, and large solvent residue, and achieve product purity and yield improvement, simplify post-processing requirements, and increase production speed Effect

Pending Publication Date: 2022-01-21
西安尚诚生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The water solubility of ecdysterone is strong, but the boiling point of water is relatively high. In many methods based on water extraction of ecdysterone, the process of concentrating the water extract has a high concentration temperature and a long concentration time, which will affect the ecdysterone adverse effects on the biological activity of
[0006] (2) In many water-based methods for extracting ecdysterone, after the separation and purification of the macroporous resin, the obtained water extract needs to be concentrated with alcohol water or acetone water. This concentration process also has a high concentration temperature, and the concentration long time problem
[0007] (3) The water solubility of ecdysterone is strong, and the extraction effect is not good, which easily leads to a greatly reduced yield. At the same time, the production wastewater contains a large amount of ecdysterone, which cannot be directly discharged to the environment, which increases the cost of wastewater treatment
However, this method involves methanol, acetone and tetrahydrofuran, and the solvent residue is large
The product can be used for veterinary breeding, but it is not suitable for higher requirements of medicine, cosmetics, etc., and the use of the product is limited

Method used

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  • Method for extracting and refining ecdysterone
  • Method for extracting and refining ecdysterone
  • Method for extracting and refining ecdysterone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] In the traditional process of extracting ecdysterone from dry dew grass, water is usually used as a solvent for extraction, because water has good solubility for ecdysterone, which can effectively extract ecdysterone in dew grass to obtain crude product. However, as described in the background art, due to the high boiling point of water, the biological activity of ecdysterone is easily destroyed due to prolonged high temperature concentration when the crude product is concentrated in this solution. In addition, the art also uses toxic solvents such as methanol or acetone to extract ecdysterone. At present, it is rare to use ethanol to directly extract ecdysterone from dried dew grass.

[0057] This example discusses whether the ultrasonic leaching method can effectively replace the heating and refluxing leaching process.

[0058] Pulverize the dried dew grass, pass through a 60 mesh sieve, take 6g and divide it into two parts, each part is 3g, one part is placed in a d...

Embodiment 2

[0061] This case mainly discusses the extraction efficiency of ecdysterone from Dewweed by different concentrations of ethanol.

[0062] Pulverize the dried dew grass, pass through a 60-mesh sieve, take a portion of 3 g, add 180 g of ethanol or different concentrations of ethanol / water solution to a distillation flask, ultrasonicate for 20 min with an ultrasonic device, take out and filter, take a small amount of filtrate and centrifuge on a centrifuge, Spin at 10,000 r / min, centrifuge for 10 min, pass the supernatants of the two through the membrane, take 1 ml of each of the supernatants into a 25 ml volumetric flask, dilute to the mark with 50% ethanol, and inject 10 microliters into the high-performance liquid phase. In the chromatograph, the detection wavelength is 243nm, and the content of ecdysterone in the two liquids is compared by the size of the chromatogram area.

[0063]

[0064] By comparison, it can be seen that when the concentration of 65%~70% ethanol is use...

Embodiment 3

[0066] On the basis of Example 2, in order to further improve the utilization rate of dew grass raw materials, this example discusses whether it is necessary to perform 2 or 3 times of leaching.

[0067] The experimental operation is as in Example 2. In this example, ethanol with a concentration of 70% is used to extract the filter residues that have undergone different extraction times.

[0068]

[0069] The results show that 2-3 times are more reasonable extraction times. When only one extraction was performed, the filter residue still contained more ecdysterone residues, and the utilization rate of dew grass was not high. However, when the extraction times exceeded 4 times, the peak area of ​​ecdysterone in the extract did not change significantly. Considering the effect of economy and impurities on the subsequent purification of ecdysterone, it was no longer necessary to re-extract the filter residue.

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Abstract

The invention discloses a method for extracting and refining ecdysterone. The method comprises the following steps: drying and crushing cyanotis arachnoidea; extracting with ethanol; filtering ; adding a ZTC1 + 1 clarifying agent into the extracting solution, stirring and precipitating, and reserving a clear liquid part; purifying the filtrate treated by the clarifying agent through a macroporous resin column; concentrating the effluent of the macroporous resin column to obtain a crude product concentrated solution; diluting the crude product concentrated solution with an organic solvent; adsorbing and purifying by using Fe3O4 magnetic nanoparticles; taking the clear liquid part to pass through a chromatographic column for chromatography; and carrying out vacuum concentration on the chromatographic solution, and carrying out vacuum freeze drying to obtain pure ecdysterone after drying. According to the method, ecdysterone with the content of 98% or above can be obtained, so that the product content is increased, the product purity and yield are greatly increased, ethyl alcohol and ethyl acetate used in the production process can be recycled according to the boiling points of ethyl alcohol and ethyl acetate, and the product extracted through the method almost has no solvent residues, is higher in purity and is safer.

Description

technical field [0001] The invention relates to the technical field of natural compound extraction, in particular to a method for extracting and refining ecdysterone. Background technique [0002] Ecdysterone, also known as ecdysone, ecdysteroids, is a class of natural steroid compounds with insect ecdysis activity. As early as 1919, biologist Polish proposed the hormone mechanism of insect ecdysis. In 1954, Butenadt and Karlson isolated α-ecdysone from silkworm pupae, and determined the steroid structure of its α, β unsaturated enone. Ecdysone is a plant steroid, so the official name should be ecdysterone. Its contents are mainly β-ecdysone (β-ecdysone), which plays a role in promoting ecdysone growth, so it can also be called ecdysone. And because its molecular structure has 20 hydrogen groups, it is also called 20-hydroxyecdysone. [0003] Ecdysone is an endogenous hormone of insects. It controls the growth and development of insects in the physiological process of ins...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 李辉何西李兵
Owner 西安尚诚生物科技有限公司
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