Preparation method for chemical reference substances of anthraquinone glucoside and stibene glucoside in rheum officinale medicinal material

A technology of stilbene glycoside chemistry and anthraquinone glycosides, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of restricting research and not being able to fully reflect the quality of rhubarb, and achieve simple operation and easy The effect of automatic control and high recovery rate

Inactive Publication Date: 2013-11-27
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

However, the chemical components currently used for the quality control of rhubarb medicinal materials and their products are 5 kinds of free anthraquinones, which are not enough to fully reflect the quality of rhubarb
Therefore, the establishment of quality control methods for various chemical components is of great significance for the comprehensive development and utilization of rhubarb medicinal materials, but the lack of anthraquinone glycosides and stilbene reference substances seriously restricts research in this area

Method used

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  • Preparation method for chemical reference substances of anthraquinone glucoside and stibene glucoside in rheum officinale medicinal material
  • Preparation method for chemical reference substances of anthraquinone glucoside and stibene glucoside in rheum officinale medicinal material
  • Preparation method for chemical reference substances of anthraquinone glucoside and stibene glucoside in rheum officinale medicinal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 The preparation method of anthraquinone glycoside and stilbene glycoside chemical reference substance in rhubarb medicinal material comprises the following steps:

[0029] (1) Extraction: After the dried root of rhubarb was crushed to 40 mesh, 500 g was taken, and 2.5 L of ethanol with a mass concentration of 10% was used for heat reflux extraction at 50°C. ; The extract was concentrated under reduced pressure at 60°C and 0.04 MPa until there was no alcohol smell, and the extract concentrate was obtained.

[0030] Among them: rhubarb dried root refers to Tangut rhubarb ( Rheum tanguticum Maxim. ex Balf.).

[0031] (2) Enrichment: put the extract concentrate on a D101 macroporous adsorption resin column, and then use 5 times the column bed volume of deionized water, ethanol with a mass concentration of 30%, ethanol with a mass concentration of 40%, and ethanol with a mass concentration of 50%. ethanol with a mass concentration of 95% ethanol, of which ...

Embodiment 2

[0038] Example 2 The preparation method of anthraquinone glycoside and stilbene glycoside chemical reference substance in rhubarb medicinal material comprises the following steps:

[0039] (1) Extraction: after crushing the dried rhubarb medicinal root to 200 mesh, take 500 g, use 15 L of ethanol with a mass concentration of 95% to carry out heat reflux extraction at 80°C, the extraction times are 3 times, each time for 3 h, and combined to obtain the extraction solution; the extract was concentrated under reduced pressure at 80°C and 0.07MPa until there was no alcohol smell, and the extract concentrate was obtained.

[0040] Among them: the dry root of rhubarb medicinal material refers to the Polygonaceae plant rhubarb palmatum ( Rheum palmatum L.) dry roots.

[0041] (2) Enrichment: put the extract concentrate on the AB-8 macroporous adsorption resin column, and use deionized water with 20 times the volume of the column bed, ethanol with a mass concentration of 30%, e...

Embodiment 3

[0048] Example 3 The preparation method of anthraquinone glycoside and stilbene glycoside chemical reference substance in rhubarb medicinal material comprises the following steps:

[0049] (1) Extraction: After crushing the dried rhubarb medicinal root to 80 mesh, take 500 g, and use 5 L of ethanol with a mass concentration of 70% to carry out heat reflux extraction at 70°C. The extraction times are 3 times, each time for 2 h, and combined to obtain the extraction solution; the extract was concentrated under reduced pressure at 70°C and 0.05 MPa until there was no alcohol smell, and the extract concentrate was obtained.

[0050] Among them: rhubarb medicinal dry root refers to medicinal rhubarb ( Rheum officinale Baill.) dry roots.

[0051] (2) Enrichment: put the extract concentrate on a D3520 macroporous adsorption resin column, and sequentially use 15 times the column bed volume of deionized water, ethanol with a mass concentration of 30%, ethanol with a mass concen...

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Abstract

The invention relates to a preparation method for chemical reference substances of anthraquinone glycoside and stibene glucoside in a rheum officinale medicinal material. The method comprises (1) a step of performing heat reflux extraction after the rheum officinale medicinal material dry root is smashed, and subjecting an extract to concentration under reduced pressure until the extract has no alcohol smell to obtain an extract concentrate; (2) a step of adding the extract concentrate to a macroporous adsorption resin column to perform elution to obtain an eluate of the target components, and subjecting the eluate to concentration under reduced pressure to constant weight to obtain a crude extract of the target components; (3) a step of separating the crude extract by utilization of HSCCC using chloroform-ethyl acetate-methanol-water as a solvent system to individually obtain aloe-emodin-8-O-beta-D-glucoside, emodin-1-O-beta-D-glucoside and emodin-8-O-beta-D-glucoside which are three anthraquinone glycoside compounds, and a stibene glucoside compound resveratrol-4'-O-beta-D-(6''-O-galloyl)-glucoside; (4) a step of purity detection, namely a step of subjecting each of the compounds separated by the HSCCC to purity detection by utilization of HPLC; and (5) a step of structure identification, namely a step of subjecting each of the compounds separated by the HSCCC to <1>H-NMR and <13>C-NMR for identification. The method is simple and fast.

Description

technical field [0001] The invention relates to a preparation method of a chemical reference substance, in particular to a preparation method of anthraquinone glycoside and stilbene glycoside chemical reference substance in rhubarb medicinal materials. Background technique [0002] Rhubarb palmatum ( Rheum palmatum L.), Tangut rhubarb ( Rheum tanguticum Maxim. ex Balf.) and medicinal rhubarb ( Rheum officinale Baill.) is a Polygonaceae plant, which is the main source of rhubarb medicinal materials. The main chemical components are tannins, phenyrophenones, stilbenes, and anthraquinones. It has strong antibacterial, antipyretic, liver protection, and blood lipid lowering properties. , Hemostasis, anti-tumor, immune regulation and other multiple functions, modern pharmacological studies have proved that anthraquinones and stilbenes are the main active ingredients. However, the chemical components currently used in the quality control of rhubarb medicinal materials and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/244C07H15/203C07H1/08
Inventor 陈涛陈晨李玉林孙菁
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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