Preparation method of pectolinarigenin monomer

A technology of iodophor and monomer is applied in the field of separation and purification of active components of traditional Chinese medicine, and achieves the effects of good reproducibility, good separation effect and strong target.

Active Publication Date: 2013-04-03
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is cumbersome and repeatedly uses petroleum ether
Because petroleum ether is flammable and explosive, the production process is very dangerous
At the same time, only the total flavonoids of thistle charcoal can be extracted by this process, and the most critical separation and purification process in the plant extraction industry is required from the total flavonoids to the rutinin monomer, which is the most technically difficult process

Method used

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  • Preparation method of pectolinarigenin monomer
  • Preparation method of pectolinarigenin monomer
  • Preparation method of pectolinarigenin monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A rapid preparation method of ruthin monomer, comprising the following process steps:

[0045] A extraction of total flavonoids

[0046] Take 100kg of thistle medicinal material, crush it into a coarse powder of 1-4mm, place it in 1m 3 In the extraction tank, add 600L of methanol with a volume fraction of 90%, heat and reflux extraction for 3 times, each extraction time is 3 hours, filter, combine the filtrates, and concentrate at 60°C to obtain about 70L of extract with a relative density of 1.1;

[0047] B hydrolyzed flavonoid glycosides

[0048] Put 70L of the concentrated extract obtained in step A into an enamel hydrolysis tank, add 0.7L of concentrated sulfuric acid to stir, heat to boiling, keep boiling for 3.5 hours for hydrolysis, and let the hydrolyzate cool to room temperature;

[0049] C Macroporous Adsorption Resin Enrichment of Flavonoids

[0050] Pass the hydrolyzate obtained in step B through the prepared AB-8 type macroporous adsorption resin column, t...

Embodiment 2

[0060] A rapid preparation method of ruthin monomer, comprising the following process steps:

[0061] A extraction of total flavonoids

[0062] Take 300kg of thistle medicinal material, crush it into a coarse powder of 1-4mm, and place it in a 3m 3 In the extraction tank, add 2400L of methanol with a volume fraction of 70%, heat and reflux for extraction 4 times, each extraction time is 2 hours, filter, combine the filtrates, and concentrate at 90°C to obtain about 250L of extract with a relative density of 1.05;

[0063] B hydrolyzed flavonoid glycosides

[0064] Put 250L of the concentrated extract obtained in step A into an enamel hydrolysis tank, add 5L of concentrated sulfuric acid to stir, heat to boiling, keep boiling for 2.5 hours for hydrolysis, and let the hydrolyzate cool to room temperature;

[0065] C Pore Adsorption Resin Enrichment of Flavonoids

[0066] Pass the hydrolyzate obtained in step B through the prepared D104 macroporous adsorption resin column with...

Embodiment 3

[0076] A rapid preparation method of ruthin monomer, comprising the following process steps:

[0077] A extraction of total flavonoids

[0078] Take 50kg of thistle medicinal material, crush it into a coarse powder of 1-4mm, and place it in 1m 3 In the extraction tank, add 400L of methanol with a volume fraction of 80%, heat and reflux for extraction 5 times, each extraction time is 1.5 hours, filter, combine the filtrates, and concentrate at 70°C to obtain about 40L of extract with a relative density of 1.0;

[0079] B hydrolyzed flavonoid glycosides

[0080] Put 40L of the concentrated extract obtained in step A into an enamel hydrolysis tank, add 1.2L of concentrated sulfuric acid to stir, heat to boiling, keep boiling for 1.5 hours for hydrolysis, and let the hydrolyzate cool to room temperature;

[0081] C Macroporous Adsorption Resin Enrichment of Flavonoids

[0082] Pass the hydrolyzate obtained in step B through the prepared D101 macroporous adsorption resin column ...

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Abstract

The invention discloses a preparation method of a pectolinarigenin monomer, and belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines. The preparation method comprises the specific process steps as follows: extracting total flavone through methanol or ethanol; adding concentrated sulfuric acid to hydrolyze flavonoid glycoside; enriching flavone in the hydrolysate through macroporous adsorptive resin; separating pectolinarigenin monomer from the stripping liquid by preparative high performance liquid chromatography; concentrating the preparation liquid under reduced pressure at 50 to 80 DEG C; standing and devitrifying; filtering; and drying to obtain the pectolinarigenin monomer product. The preparation method is simple and convenient in operation, short in production period, high in separation efficiency, stable in process and low in cost, and can realize industrial separation and preparation of a high-purity pectolinarigenin monomer, so that the pectolinarigenin monomer with purity more than 99% can be obtained.

Description

technical field [0001] The invention relates to a preparation method of a plant compound monomer, in particular to a method for extracting and isolating the ruthin monomer from euphemum medicinal material, and belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines. [0002] Background technique [0003] Liuchuanyu is mainly derived from the Chinese herbal medicine thistle, which is a plant of the genus Thistle in the family Asteraceae. Cirsium japonicum Dry aerial parts of Fisch. ex DC. As thistle contains a variety of flavonoids and glycosides, it has obvious effects of cooling blood, stopping bleeding, dispelling blood stasis and detoxifying. Among them, the flavonoids with the highest content are the flavonoids of scutellaria japonicus and its aglycon scutellaria lutein, and the 2010 edition of the Pharmacopoeia of the People's Republic of China recorded scutellaria lutein as the identification index compone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30
Inventor 夏柯李启发文焕松郭建华刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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