Novel method for extracting and separating high purity tiliroside from edgeworthia chrysantha

A high-purity, new method technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of poor product quality, large sample loss, solvent residue, etc., and achieve small sample loss and separation time. Short, strong separation effect

Inactive Publication Date: 2012-01-11
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chen Gang used 10 times the amount of industrial alcohol to cold-soak for a week in his master's thesis "Research on the Chemical Composition of Yujin and Wenyujin". , and then separated by silica gel column crude separation, Sephadex LH-20 column chromatography, high-speed countercurrent chromatography purification and other steps to obtain the components, and separated with n-hexane-ethyl acetate-methanol-water (3:7:4:6) solvent system Obtain silver satin, this method passes through column chromatography for many times, and sample loss is bigger
Chinese Patent (Publication No. CN1733788A) "A Method for Extracting and Separating Silver Lindensin from Jasmine Flower", using 60-100% methanol or ethanol solution for leaching or reflux extraction, the extract is washed with water and then reflux extraction with a fat-soluble solvent to obtain The filter cake is recrystallized to obtain products, and toxic organic solvents are used, resulting in solvent residues and poor product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 2kg of jiexianghua and crush it through a 10-mesh sieve, add 5 times the amount of 70% ethanol for ultrasonic extraction for 1 hour, extract 3 times, combine the extracts, first use a vibrating screen filter to continuously filter out physical impurities such as sediment, and then use a hollow polymer For propylene ultrafiltration membrane concerns, add 2% activated carbon to the permeate to stir for decolorization. The decolorization solution is concentrated under reduced pressure to no alcohol, dispersed with water, added to AB-8 macroporous adsorption resin column for adsorption, first eluted with 4BV30% ethanol, and then 5BV75 % ethanol to elute the effective components, collect the target components, concentrate under reduced pressure, centrifuge, and dry the centrifugate to obtain 24g of crude extract.

[0015] Mix ethyl acetate, n-butanol, and water in a ratio of 5:2:5, let stand and separate, and ultrasonically degas the two phases respectively for 30 minute...

Embodiment 2

[0017] Take 2kg of Jiexiang flower and crush it through a 20-mesh sieve, add 4 times the amount of 60% ethanol for ultrasonic extraction for 2 hours, extract 3 times, combine the extracts, first use a vibrating screen filter to continuously filter out physical impurities such as sediment, and then use a hollow polymer For the concerns of vinylidene fluoride ultrafiltration membrane, add 4% activated carbon to the permeate to stir for decolorization. The decolorization solution is concentrated under reduced pressure until alcohol-free, dispersed with water, added to AB-8 macroporous adsorption resin column for adsorption, first eluted with 5BV40% ethanol, and then The effective components were eluted with 4BV80% ethanol, the target components were collected, concentrated under reduced pressure, centrifuged, and the centrifugate was dried to obtain 22 g of crude extract.

[0018] Take n-hexane, n-butanol, methanol, and water and mix them in a ratio of 1:4:2:5, let them stand for ...

Embodiment 3

[0020] Take 5 kg of Jiexiang flower and crush it through a 20-mesh sieve, add 5 times the amount of 80% methanol for ultrasonic extraction for 1.5 hours, extract twice, combine the extracts, first use a vibrating screen filter to continuously filter out physical impurities such as sediment, and then use a hollow polymer For ether sulfone ultrafiltration membrane concerns, add 3.5% activated carbon to the permeate and stir to decolorize. The decolorized solution is concentrated under reduced pressure to no alcohol, dispersed with water, added to AB-8 macroporous adsorption resin column for adsorption, first eluted with 3BV30% ethanol, and then 5BV80% ethanol elutes the effective components, collects the target components, concentrates under reduced pressure, centrifuges, and dries the centrifugate to obtain 56 g of crude extract.

[0021] Mix n-hexane, ethyl formate, acetonitrile, and water in a ratio of 5:5:2:4, let stand and separate, and ultrasonically degas the two phases re...

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PUM

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Abstract

The invention relates to a novel method for extracting and separating high purity tiliroside from edgeworthia chrysantha. The method comprises the steps of extraction, ultrafiltration, decolouring, macroporous resin column chromatography, separation and extraction by using the technology of high speed counter current chromatography, condensation, drying and the like so as to separate and prepare high purity tiliroside. According to the invention, a process for extracting tiliroside is stable; the content of tiliroside in the obtained product in the invention is high and is more than 97% according to determination of the technology of high speed counter current chromatography.

Description

technical field [0001] The invention belongs to a method for extracting and purifying active ingredients of traditional Chinese medicines, and in particular relates to a new method for extracting and separating high-purity tidalin from jacaranda. Background technique [0002] Aroma is a plant of the genus Edgeworthia of Thymelaeaceae (Thymelaeaceae) Edgeworthia chrysantha , produced in Henan, Shaanxi and the provinces south of the Yangtze River Basin, the stem bark fiber can be used as raw materials for high-grade paper and artificial cotton. Folks often use the fragrant root and flower as medicine, and the flower is often used as a substitute for Budisma japonica, which has the effects of nourishing yin and calming the nerves, improving eyesight, and removing obscuration. ,aphonia. There are literatures on the isolation of coumarin, flavonoids, organic acids, nitrogen heterocycles and other compounds from A. japonica. [0003] Tiliroside, yellow needle crystal, mp.215-21...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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