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Method for preparing high-purity monomer of cholest-4-olefin-3-ketone in syngnathus schlegeli

A high-purity, sea dragon technology, applied in the direction of steroids, organic chemistry, etc., can solve the problem that the extraction and separation purity cannot meet the performance requirements of the standard product, and achieve the effect of complete extraction, large extraction amount, and easy storage

Inactive Publication Date: 2013-12-18
THE FIRST INST OF OCEANOGRAPHY SOA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] For this reason, the technical problem to be solved by the present invention lies in the problem that the extraction and separation purity of cholest-4-en-3-one in the prior art cannot meet the performance requirements of the standard product, and then provides a method for preparing the high-purity Cholester 4-en-3-one method

Method used

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  • Method for preparing high-purity monomer of cholest-4-olefin-3-ketone in syngnathus schlegeli
  • Method for preparing high-purity monomer of cholest-4-olefin-3-ketone in syngnathus schlegeli
  • Method for preparing high-purity monomer of cholest-4-olefin-3-ketone in syngnathus schlegeli

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Embodiment 1

[0057] The method for preparing the high-purity monomer of cholest-4-en-3-one in Hailong described in this embodiment comprises the following steps:

[0058] (1) Take 10 g of the coarse powder of sea dragon and grind it through a 200-mesh sieve to obtain the dry powder of sea dragon, and use 95% ethanol for immersion and extraction for 5 hours, and heat and concentrate to the extract to obtain the initial body of the extract;

[0059] (2) Place the initial body of the extract in a Soxhlet extractor, add 150 mL of n-hexane to reflux and extract for more than 6 hours, recover the solvent to obtain the n-hexane extract, and concentrate to obtain the extract;

[0060] (3) Add 20 mL of 10% KOH-ethanol solution to the extract, shake vigorously for 2 min, put it in a water bath at 65° C. for saponification, shake once every 15 min, and react for 1 h after the solution is clarified to obtain a saponified product;

[0061] (4) Add 20ml of distilled water to the saponified product for ...

Embodiment 2

[0105] The method for preparing cholest-4-en-3-one monomer in the present embodiment is the same as that in embodiment 1, and its difference is that in step (5), the developing system used is n-butanol: acetic acid: the ratio of water is 4:1:5, the TLC pattern of the sample is as follows Figure 8 Shown in B.

Embodiment 3

[0107] The method for preparing cholest-4-en-3-one monomer in the present embodiment is the same as that in Example 1, the only difference being that in step (5), the development system used is n-butanol: isoamyl alcohol: water The ratio is 2:1:1, the TLC pattern of the sample is as follows Figure 8 Shown in C.

[0108] From Figure 8 Middle A, Figure 8 Medium B and Figure 8 From the results shown in C, it can be seen that the thin-layer chromatography of sterols with the development system of the present invention has clearer bands and better separation effects.

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Abstract

The invention belongs to the field of biology purification, and particularly relates to a method for extracting cholest-4-olefin-3-ketone in syngnathus schlegeli and preparing high-purity monomer of the cholest-4-olefin-3-ketone. The method for extracting cholest-4-olefin-3-ketone in syngnathus schlegeli comprises the following steps of: steeping and primarily extracting, saponifying, performing chromatography, extracting, crystallizing sequentially to obtain the high-purity cholest-4-olefin-3-ketone with the purity up to more than 99% which achieves the requirement on preparing standard products. The stability of samples is better.

Description

technical field [0001] The invention belongs to the field of biological purification, and in particular relates to a method for extracting cholest-4-en-3-one from sea dragon and preparing its high-purity monomer. Background technique [0002] Sea dragon belongs to chordate phylum Osteichthyes, Syngnathiformes, and Syngnathidae. It is a very important marine animal traditional Chinese medicine. It also has physiological functions such as improving the body's immunity and enhancing the contractility of cardiomyocytes. [0003] Modern biochemical and pharmacological studies have shown that the drug effect of sea dragon is closely related to the contained sterols, but there are few studies on the active ingredients in sea dragon, especially the sterols in the prior art. This is due to the fact that the sterols Although it is a beneficial component, its content is small, and the difficulty of extracting and separating sterol components has also become a bottleneck restricting fu...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 丛柏林沈继红靳永轩黄晓航刘胜浩
Owner THE FIRST INST OF OCEANOGRAPHY SOA
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