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Method for preparing calycosin-7-O-beta-D-glucoside and ononin chemical reference products synchronously

A technology of verbascoside and reference substance, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of cumbersome process, large recrystallization loss, and unresearched preparation of verbascoside and formononetin. See literature reports and other issues to achieve the effect of simple process and high yield

Inactive Publication Date: 2011-05-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] At present, there are few reports on the preparation of flavonoid glycosides from Astragalus membranaceus. Chinese patent (CN00710176318.5) reports the use of extraction, resin chromatography enrichment and repeated recrystallization to obtain verbascoisoflavone glycosides with a purity of about 97%. The number of times is 5-7 times, the process is more cumbersome and the recrystallization loss is larger
However, there is no literature report on the preparation of large-scale acteocoside and formononetin at the same time.

Method used

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  • Method for preparing calycosin-7-O-beta-D-glucoside and ononin chemical reference products synchronously
  • Method for preparing calycosin-7-O-beta-D-glucoside and ononin chemical reference products synchronously
  • Method for preparing calycosin-7-O-beta-D-glucoside and ononin chemical reference products synchronously

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Silica gel column chromatography enrichment:

[0028] Astragalus ethanol extract 100g, separated by silica gel decompression chromatography (21cm*12cm), eluted with ethyl acetate:methanol (9:1) of 5 times the column volume, 500ml of each fraction was collected, and detected by thin layer chromatography, in which the developer Ethyl acetate: methanol: water (9: 1: 0.5), the color developer is a sulfuric acid ethanol solution with a volume concentration of 5%, and the fractions with an Rf value of 0.4-0.6 are combined and dried under reduced pressure to obtain 750 mg of a brown powder ( figure 1 );

[0029] 2) Resin column removal of impurities:

[0030] The tan powder is dissolved with 10% ethanol solution, filtered through four layers of gauze, and the supernatant liquid is separated on a HPD-100 resin column, wherein the sample: the resin ratio is 1: 6 (g: ml), respectively with 5 times the column volume of water, 25 % ethanol solution, 45% ethanol solution for el...

Embodiment 2

[0034] 1) Silica gel column chromatography enrichment:

[0035] Astragalus ethanol extract 1000g, separated by silica gel column chromatography (8cm*80cm), eluted with ethyl acetate:methanol (8:2) of 4 times the column volume, 500ml of each fraction is collected, and detected by thin-layer chromatography, wherein the developer is Ethyl acetate: methanol: water (9:1:0.5), the developer is 5% sulfuric acid ethanol solution, the fractions with Rf value of 0.4-0.6 are combined, and dried under reduced pressure to obtain 7.4 g of brown powder;

[0036] 2) Resin column removal of impurities:

[0037] The brownish yellow powder was dissolved with 25% ethanol solution, filtered through four layers of gauze, and the clear liquid was separated on a Diaion resin column, wherein the sample: resin ratio was 1:5 (g:ml), and the water and 30% ethanol were used for 4 times the column volume respectively. solution and 50% ethanol solution, respectively collected 30% ethanol eluate, concentrat...

Embodiment 3

[0041] 1) Silica gel column chromatography enrichment:

[0042] Astragalus ethanol extract 2000g, separated by silica gel column chromatography (9.5cm*120cm), eluted with 3 times column volume of ethyl acetate:methanol (7:3), 500ml of each fraction was collected, and detected by thin layer chromatography, in which the developer Ethyl acetate: methanol: water (9:1:0.5), the developer is 5% sulfuric acid ethanol solution, the fractions with Rf value of 0.4-0.6 are combined, dried under reduced pressure to obtain 15 g of brown powder;

[0043] 2) Resin column removal of impurities:

[0044] The tan powder was dissolved with 10% ethanol solution, filtered through four layers of gauze, and the supernatant liquid was separated on a HPD-100 resin column, wherein the sample: the resin ratio was 1: 6 (g: ml), and 3 times the column volume of water, 35 % ethanol solution and 55% ethanol solution for elution, respectively collected 35% ethanol eluate, concentrated and dried to obtain 3....

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Abstract

The invention relates to novel process for preparing calycosin-7-O-beta-D-glucoside and ononin chemical reference products synchronously. The calycosin-7-O-beta-D-glucoside and ononin chemical reference products with a purity of over 98 percent can be obtained by purifying alcohol extract of astragalus by silica gel column chromatography, resin column impurity removal and preparation of high performance liquid chromatography. In the invention, the process steps are simple, the purity is high, the color and luster are desirable, and large-scale production is easy.

Description

[0001] Technical field The present invention relates to a new process for preparing chemical reference substances of Calycosin-7-O-β-D-glucoside and Ononin simultaneously. It mainly includes three-step purification of silica gel column chromatography enrichment, resin column impurity removal and reversed-phase high performance liquid phase preparative chromatography. 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. Actascoside and formononetin are two flavonoid glycosides with high content in Astragalus membranaceus. The 2010 edition of Chinese Pharmacopoeia has included actcocoside as one of the quality control index components of Astragalus membranaceus. Due to the high polarity of this compound, it is d...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/07
Inventor 肖红斌王莉彭杰卓荣杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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