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Method for extracting herbacetin from rhodiola rosea

A technology of oxalanthin and Rhodiola rosea, applied in the fields of chemistry and medicinal chemistry, can solve the problems of less oxalanthin and undisclosed process route of high-purity oxalool, achieve easy elution and regeneration, long elution cycle, The effect of good separation

Active Publication Date: 2017-08-18
TAIZHOU DANDING BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, there are few research reports on herbal extracts, and there is no disclosure of a process route suitable for industrial production to prepare high-purity herbal extracts

Method used

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  • Method for extracting herbacetin from rhodiola rosea
  • Method for extracting herbacetin from rhodiola rosea
  • Method for extracting herbacetin from rhodiola rosea

Examples

Experimental program
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Effect test

specific Embodiment 1

[0046] Weigh 20kg of Tibet-produced Rhodiola rosea (detected by high-performance liquid chromatograph, herbaceous-7-O-rhamnoside, herbaceous-7-O-(3″-β-D-glucosyl)-rhamnoside The contents of glycosides are 0.12% and 0.11%, respectively, and the liquid phase detection chromatogram of the medicinal material is shown in image 3 , the detection chromatogram after acid hydrolysis is shown in Figure 4 ), crushed through a 20-mesh sieve, heated and refluxed with 10 times the mass fraction of 70% ethanol solution for 2 times, each 1.5h, combined the extracts and concentrated under reduced pressure to obtain the ethanol extract extract (relative density is 1.072), Extract 3 times with the petroleum ether (60-90 ℃) equal volume of ethanol extract extract, add equal volume mass fraction to the aqueous layer after the extraction is the ethyl acetate of 1% sulfuric acid and 2 times extract volume, Stir, heat and reflux to carry out two-phase acid hydrolysis treatment, hydrolyze for 12h, ...

specific Embodiment 2

[0048] Take by weighing 80kg Jilin Changbai Mountain to produce Alpine Rhodiola rosea (through the high-performance liquid chromatograph detection herbaceous element-7-O-rhamnoside, herbaceous element-7-O-(3″-β-D-glucosyl)- The contents of rhamnoside are respectively 0.067% and 0.028%. Figure 5 , the detection chromatogram after acid hydrolysis is shown in Image 6 ), pulverized through a 20 mesh sieve, percolated and extracted with 12 times the amount of 90% ethanol solution, the percolated liquid was concentrated under reduced pressure to obtain the ethanol extract extract, and the combined extract was concentrated under reduced pressure to obtain the ethanol extract extract (relative density is 1.136), extract 3 times with petroleum ether (60-90° C.) equal to the volume of the ethanol extract extract, add 5% hydrochloric acid to the aqueous layer after the extraction, and then add 2 times the extract volume ethyl acetate, stirred, heated to reflux for acid hydrolysis for ...

specific Embodiment 3

[0050] Weigh 10kg of Rhodiola rosea produced in Lijiang, Yunnan (through high-performance liquid chromatography to detect herbalanin-7-O-rhamnoside, herbalanin-7-O-(3″-β-D-glucosyl)-ratine The contents of glucoside are respectively 0.10% and 0.10%), crushed through a 20-mesh sieve, ultrasonically extracted 3 times with 12 times the mass fraction of 90% methanol solution, 1 hour each time, combined the extracts and concentrated under reduced pressure to obtain the methanol extract Extract (relative density is 1.025), extract 3 times with petroleum ether (60-90°C) equal to 3 times the volume of methanol extract extract, add an equal volume of hydrochloric acid with a mass fraction of 1% to the extracted water layer , stirred, heated to reflux for acid hydrolysis treatment, hydrolyzed for 1h, cooled, added petroleum ether-ethyl acetate (1:1) to the hydrolyzed solution for extraction 5 times, each time the amount of petroleum ether-ethyl acetate (1:1) The ratio of the hydrolyzate ...

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Abstract

A method for extracting herbacetin from rhodiola rosea comprises the steps of: 1) extracting a medicinal material by using an extraction solvent, and then concentrating to obtain an extract paste; 2) extracting the extract paste, and acid hydrolyzing an aqueous layer obtained from the extraction; 3) extracting a solution obtained from the acid hydrolysis with an organic solvent, combining with the extraction solution, concentrating under reduce pressure to obtain an extract of herbacetin; 4) treating the extract of herbacetin with polyamide column chromatography, collecting fractions containing herbacetin, concentrating till dry, and recrystallizing to obtain a pure product of herbacetin.

Description

technical field [0001] The invention relates to a method for separating and extracting compounds in the field of chemistry, in particular to a method for preparing herbalin from rhodiola rosea, and belongs to the field of medicinal chemistry. Background technique [0002] The genus Rhodiola in the Sedum family is a perennial herb or subshrub. There are more than 90 species of Rhodiola in the world, and 73 species in my country. Among the many species of Rhodiola plants, domestic and foreign scholars mainly focus on more than ten Rhodiola rosea, Rhodiola rosea, Rhodiola small clusters, Rhodiola sakhalin, Rhodiola angustifolia and Rhodiola holy land. type. The chemical composition of Rhodiola rosea varies greatly from species to species, as do their effects. Rhodiola rosea recorded in the 2015 edition of "Chinese Pharmacopoeia" is the dry root and rhizome of Rhodiola grandiflora, a plant of the sedum family. It is used for qi deficiency and blood stasis, chest obstruction a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40A61K2236/00A61K31/352A61K36/41
Inventor 顾正兵张杰陶月红曾铖徐丽丽
Owner TAIZHOU DANDING BIOTECH CO LTD
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