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Method for simultaneously preparing chemical reference substances of calycosin and formononetin

A technology of calycosin and formononetin, applied in the direction of organic chemistry, can solve the problems of cumbersome steps and low purity of reference substances, and achieve the effect of simple process

Inactive Publication Date: 2013-02-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most of the reports on the preparation of flavonoids from Astragalus are laboratory-scale, and the steps are cumbersome; there are a small number of large-scale production reports, but the purity of the reference substance is not high

Method used

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  • Method for simultaneously preparing chemical reference substances of calycosin and formononetin
  • Method for simultaneously preparing chemical reference substances of calycosin and formononetin
  • Method for simultaneously preparing chemical reference substances of calycosin and formononetin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Silica gel column chromatography enrichment:

[0026] Astragalus alcohol extract extract 70g, add about 70g silica gel and mix well, dry under reduced pressure at 60°C, separate by silica gel vacuum chromatography (21cm*12cm), use 5 times of column volumes of petroleum ether: ethyl acetate (volume ratio 8 : 2), petroleum ether: ethyl acetate (volume ratio 7: 3), petroleum ether: ethyl acetate (volume ratio 5: 5) step gradient elution, thin-layer chromatography detection, with petroleum ether: ethyl acetate (volume Ratio 1:1) as developer, GF254 fluorescent plate, dark spots were inspected at 254nm of ultraviolet light, the eluate with Rf value of 0.13 was collected, concentrated, and 35mg of light yellow precipitate was separated out (the crude product of calycosin, figure 1 ); collect the eluent whose Rf value is 0.44, concentrate, and separate out light yellow precipitate 11mg (the crude product of formononetin, figure 2 );

[0027] 2) Recrystallization:

[00...

Embodiment 2

[0031] 1) Silica gel column chromatography enrichment:

[0032] Astragalus ethanol extract extract 700g, add about 700g silica gel and mix well, dry under reduced pressure at 60°C, separate by silica gel column chromatography (8cm*80cm), use 4 times the column volume of petroleum ether: ethyl acetate (volume ratio 8: 2), petroleum ether: ethyl acetate (volume ratio 7: 3), petroleum ether: ethyl acetate (volume ratio 5: 5) step gradient elution, thin-layer chromatographic detection, with petroleum ether: ethyl acetate (volume ratio 3:7) as developer, GF254 fluorescent plate, dark spots were inspected at 254nm of ultraviolet light, the eluate with Rf value of 0.32 was collected, concentrated, and 360 mg of pale yellow precipitate (crude product of calycosin) was separated out; the eluate with Rf value of 0.64 was collected Deliquified, concentrated, and 105 mg of light yellow precipitate (crude formononetin) was precipitated;

[0033] 2) Recrystallization:

[0034] The crude p...

Embodiment 3

[0036] 1) Silica gel column chromatography enrichment:

[0037] Astragalus ethanol extract extract 7000g, add about 7000g silica gel and mix well, dry under reduced pressure at 60°C, separate by silica gel column chromatography (9.5cm*120cm), use 3 times the column volume of petroleum ether: ethyl acetate (volume ratio 8 : 2), petroleum ether: ethyl acetate (volume ratio 7: 3), petroleum ether: ethyl acetate (volume ratio 5: 5) step gradient elution, thin-layer chromatography detection, with petroleum ether: ethyl acetate (volume Ratio 1:1) as developing agent, GF254 fluorescent plate, dark spots were inspected at 254nm of ultraviolet light, the eluate with Rf value of 0.20 was collected, concentrated, and 3.58g of light yellow precipitate (crude product of calycosin) was precipitated; the collected Rf value was 0.48 The eluent was concentrated, and 1.1 g of a light yellow precipitate (crude formononetin) was separated out;

[0038] 2) Recrystallization:

[0039] The crude p...

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Abstract

The invention relates to a novel process for simultaneously preparing chemical reference substances of calycosin and formononetin, comprising two steps of purifying astragalus root alcohol extracts by utilizing silicagel column chromatography and recrystallizing to obtain the two types of chemical reference substances of the calycosin and the formononetin with purities greater than 98%. The method has the advantages of simple process steps and high purity of obtained products, and is easy for scale production.

Description

[0001] Technical field The present invention relates to a new process for the simultaneous preparation of Calycosin and Formononetin chemical reference substances. It mainly includes two steps of silica gel column chromatography purification and recrystallization. Background technique [0002] Astragalus membranaceus is a commonly used clinical traditional Chinese medicine. It has the functions of invigorating qi and raising yang, strengthening the surface and antiperspirant, diuresis and reducing swelling. The saponins and flavonoids contained in it are the main active ingredients. Calycocosin and formononetin are two isoflavone compounds with high content in Astragalus membranaceus, and they are potential quality control index components of Astragalus membranaceus. Therefore, obtaining a large number of reference substances is of great significance for the quality control of Astragalus-related products and the in-depth study of the efficacy of Astragalus. [0003] At presen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/36C07D311/40
Inventor 肖红斌王莉彭杰赵楠
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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