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A method for the separation and preparation of petrogin chemical reference substance in black saxifrage

A technology of petogenin and black saxifrage, which is applied in the field of natural medicinal chemistry, can solve the problems that have not been reported in the literature and have not been systematically researched, and achieve the effects of easy operation, suitable for large-scale production, and low cost

Active Publication Date: 2022-03-15
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are no literature reports on the large-scale and rapid preparation of the compound petracenin from black saxifrage, and the existing research has not been systematic.

Method used

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  • A method for the separation and preparation of petrogin chemical reference substance in black saxifrage
  • A method for the separation and preparation of petrogin chemical reference substance in black saxifrage
  • A method for the separation and preparation of petrogin chemical reference substance in black saxifrage

Examples

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Effect test

Embodiment 1

[0026] A method for the separation and preparation of a chemical reference substance for petracenin in saxifrage, the method specifically comprising the following steps:

[0027] Step 1, extraction: take 180g of black saxifrage and dry it in the shade, add methanol 10 times its mass after crushing, extract 3 times at room temperature, 2 hours each time, filter and combine the filtrates, namely filtrate A, the filtrate A is based on polyamide The amount: the amount of black saxifrage medicinal material = 1:15 mixed samples and dried under reduced pressure to obtain 258 g mixed samples of black saxifrage methanol extract, wherein the conditions of reduced pressure drying were vacuum degree 50 mbar, temperature 40°C;

[0028] Step 2, polyamide column enrichment: the mixed sample of the black saxifrage methanol extract, the sample is separated by a medium-pressure chromatographic column equipped with polyamide material, detected by an ultraviolet detector with a detection waveleng...

Embodiment 2

[0031] A method for the separation and preparation of a chemical reference substance for petracenin in saxifrage, the method specifically comprising the following steps:

[0032] Step 1, extraction: take 500g of black saxifrage and dry it in the shade, add methanol 10 times its mass after crushing, extract 3 times at room temperature, 3 hours each time, filter and combine the filtrates, namely filtrate A, the filtrate A is based on polyamide The amount: the amount of black saxifrage medicinal material = 1:5 mixed sample and dried under reduced pressure to obtain 270g mixed sample of black saxifrage methanol extract, wherein the conditions of reduced pressure drying are vacuum degree 250 mbar, temperature 60 ℃;

[0033] Step 2, polyamide column enrichment: the mixed sample of the black saxifrage methanol extract, the sample is separated by a medium-pressure chromatographic column equipped with polyamide material, detected by an ultraviolet detector with a detection wavelength o...

Embodiment 3

[0036] A method for the separation and preparation of a chemical reference substance for petracenin in saxifrage, the method specifically comprising the following steps:

[0037]Step 1, extraction: take 1200 g of saxifrage and dry it in the shade, add methanol 10 times its mass after crushing, extract 3 times at room temperature, each time for 4 h, filter and combine the filtrates, i.e. filtrate A, the filtrate A is obtained by polymer The amount of amide: the amount of black saxifrage medicinal material = 1:8 mixed sample and dried under reduced pressure to obtain 970g mixed sample sample of black saxifrage methanol extract, wherein, the condition of reduced pressure drying is vacuum degree 150 mbar, temperature 50°C;

[0038] Step 2, polyamide column enrichment: the mixed sample of the black saxifrage methanol extract, the sample is separated by a medium-pressure chromatographic column equipped with a polyamide material, detected by an ultraviolet detector with a detection w...

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Abstract

The invention relates to the technical field of natural medicine chemistry, in particular to a method for separating and preparing a chemical reference substance of petracenin in saxifrage. Its preparation method includes three steps: extraction, polyamide column enrichment and microporous resin column separation. The present invention has low cost and product purity greater than 98%; the technical means adopted in the present invention can be used for large-scale production: the requirements for raw materials are not high, the cost is low, and it is easy to prepare materials in batches; the methanol is extracted by cold soaking at room temperature, and it is easy to operate; the polyamide column is used for enrichment , the separation material can be installed in a medium-pressure column system and connected to the preparative liquid chromatography, which is easy to scale; the microporous resin column used in the separation is a rapid isocratic method.

Description

technical field [0001] The invention relates to the technical field of natural medicine chemistry, in particular to a method for separating and preparing a chemical reference substance of petracenin in saxifrage. Background technique [0002] Black saxifrage ( Saxifraga atrata ) belongs to the genus Saxifrage ( Saxifraga L. ), Saxifragaceae ( Saxifragaceae )plant. Modern studies have shown that the chemical components in saxifrage plants mainly include phenols and flavonoids. Modern pharmacological studies have shown that saxifrage plants (including black saxifrage) have various pharmacological effects, such as heat-clearing, detoxifying, anti-inflammatory, liver-clearing, gall-heat syndrome, and can treat rubella, eczema, otitis media, erysipelas , cough and vomiting blood, hemorrhoids and other diseases. In order to speed up the evaluation of germplasm resources of black saxifrage and the research and development of related new drugs, it is particularly important to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 高庆波迟晓峰马小磊曹倩
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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