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Method for separating reference substance of ergosterol and stellasterol from traditional Chinese medicine polyporus umbellatus

A technology for ergosterol and starfish sterol, which is applied in the directions of organic chemistry, steroids, organic chemistry, etc., can solve the problems of low sample purity, complicated operation, lengthy steps, etc., and achieves high separation difficulty, simple steps, and easy operation. Effect

Active Publication Date: 2017-09-29
GUANGDONG HOSPITAL OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The methods reported in the literature all use a variety of organic solvent extraction and a variety of fillers for column chromatography for separation and purification. There is no reference to the reference substance preparation method of ichthysterol

Method used

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  • Method for separating reference substance of ergosterol and stellasterol from traditional Chinese medicine polyporus umbellatus
  • Method for separating reference substance of ergosterol and stellasterol from traditional Chinese medicine polyporus umbellatus
  • Method for separating reference substance of ergosterol and stellasterol from traditional Chinese medicine polyporus umbellatus

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Experimental program
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Effect test

Embodiment 2

[0056] A method for isolating ergosterol and astral sterol reference substances from the traditional Chinese medicine Polyporus polyporus, comprising the following steps:

[0057] 1. Separation of ergosterol and astral sterol

[0058] Weigh 300g of dried Polyporus chinensis, crush it through a No. 3 medicine sieve, heat and reflux extraction with 5 times the amount of 98% methanol (1.5L) for 3 times, recover methanol, and obtain 15.2g of Polyporus umbilical extract, which is prepared by adding 50mL of distilled water Disperse the solution; extract the resultant three times with equal volume of petroleum ether, each time using 50 mL of petroleum ether, then extract three times with chloroform, each time using 50 mL of chloroform; finally concentrate the chloroform extract to extract;

[0059] (2) Elute the extract obtained in the previous step with 30 mL of distilled water for 3 times, filter to remove larger impurities, collect the filter residue, and filter the residue throug...

Embodiment 3

[0066] A method for isolating ergosterol and astral sterol reference substances from the traditional Chinese medicine Polyporus polyporus, comprising the following steps:

[0067] One, separate ergosterol and star fish sterol, concrete steps are:

[0068] Weigh 300g of dried Polyporus chinensis, crush through No. 3 medicine sieve, heat and reflux extraction with 8 times the amount of 95% ethanol (2.4L) for 3 times; recover methanol to obtain 14.7g of Polyporus umbilical extract, add 50mL of distilled water to make Disperse the solution; first extract the resultant three times with equal volume of petroleum ether, each time using 50 mL of petroleum ether, then extract three times with dichloromethane, each time using 50 mL of dichloromethane, and finally concentrate the chloroform extract to extract;

[0069] (2) The extracted extract obtained in the previous step was eluted 3 times with 40 mL of distilled water, filtered to remove larger impurities, and the filter residue was co...

Embodiment 4

[0076] A method for isolating ergosterol and astral sterol reference substances from the traditional Chinese medicine Polyporus polyporus, comprising the following steps:

[0077] One, separate ergosterol and star fish sterol, concrete steps are:

[0078] Weigh 5000g of dried Polyporus chinensis, crush through No. 2 medicine sieve, and extract 3 times with 3 times the amount of 98% methanol (15L) by cold immersion; recover methanol to obtain 101.7g of Polyporus umbilical extract, add 1000mL of distilled water to make a dispersion solution; the resultant was first extracted three times with equal volumes of petroleum ether, each time using 1000 mL of petroleum ether, and then extracted three times with dichloromethane, each time using 1000 mL of dichloromethane; finally concentrated the chloroform extract to extract;

[0079] (2) The extracted extract obtained in the previous step was eluted 3 times with 500 mL of distilled water, filtered to remove larger impurities, and the f...

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Abstract

The invention discloses a method for separating a reference substance of ergosterol and stellasterol from a traditional Chinese medicine polyporus umbellatus. According to the method, high-purity monomeric compounds of the ergosterol and the stellasterol are prepared from polyporaceae polyporus polyporus(pers.) dry sclerotoids, serving as raw materials, by means of ethanol liquid extraction, petroleum ether decontamination, dichloromethane extraction, sephadex LH-20 column chromatography, re-crystallization and half-preparation. The method is simple and reliable, the raw materials are easy to obtain, the economic cost is low, the specificity is strong, and the method is applicable to large-scale preparation of the reference substance of the ergosterol and the stellasterol; moreover, during extraction and crystallization, ethyl alcohol or methyl alcohol is adopted to reduce the environmental pollution, and the solvent cost is low; by means of the crystallization or preparation method, the separation and purification time of a sample is shortened, the costs of manpower and material resources are reduced, and the economic effect is improved; a reference substance for content determination can be provided for quality control over crude drugs of the traditional Chinese medicine polyporus umbellatus, thus contributing to establishment of a quality control method for the crude drugs polyporus umbellatus.

Description

technical field [0001] The invention relates to the technical field of separation and purification of traditional Chinese medicines and natural products, in particular to a method for separating ergosterol and star sterol reference substances from the traditional Chinese medicine Polyporus polyporus. Background technique [0002] Polyporus polyporus (pers.) is a dry sclerotium of the medicinal fungus Polyporaceae Polyporaceae. It is distributed in most of my country and is mainly produced in Gansu, Shaanxi, Shanxi, Henan, Sichuan, and Hunan. , Yunnan, Jilin and Heilongjiang and other places, among which Shaanxi is the most authentic. Polyporus is first recorded in "Shen Nong's Materia Medica", and is listed as a middle grade. There are relatively detailed records in "Bielu of Famous Doctors", "Zheng Lei Materia Medica" and "Compendium of Materia Medica". The traditional medicine of the motherland believes that it has "the effect of promoting water and expelling dampness", "...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07J9/00C07B2200/07Y02A50/30
Inventor 曾星谭庆龙黎雄
Owner GUANGDONG HOSPITAL OF TRADITIONAL CHINESE MEDICINE
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