Method for separating and preparing high purity flavonoid glycoside compounds from actinidia valvata dunn leaves

A technology for flavonoid glycosides from kiwifruit leaves and flavonoids is applied in the field of separating and preparing high-purity flavonoid glycosides from kiwifruit leaves, which can solve the problems of decreasing sample recovery rate, polluting the environment, laborious and laborious separation by column chromatography, and the like. Achieve the effect of large preparation amount, high recovery rate and overcoming long separation cycle

Active Publication Date: 2012-08-01
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The separation of the above three compounds by traditional column chromatography is time-consuming and laborious, pollutes the environment, and the fixed relative sample used will have irreversible adsorption, resulting in defects such as a decrease in the recovery rate of t

Method used

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  • Method for separating and preparing high purity flavonoid glycoside compounds from actinidia valvata dunn leaves
  • Method for separating and preparing high purity flavonoid glycoside compounds from actinidia valvata dunn leaves
  • Method for separating and preparing high purity flavonoid glycoside compounds from actinidia valvata dunn leaves

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Experimental program
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Effect test

Embodiment 1

[0030]1. Medicinal material extraction: Weigh 600 g of kiwifruit leaves, reflux extraction with 6 times volume concentration of 70% ethanol twice, each time for 2 hours, filter, combine filtrates, concentrate under reduced pressure at 50°C until no alcohol smell, and obtain Concentrated extract.

[0031] 2. Preparation of crude extract: Take 1000ml of the concentrated extract, add an equal amount of water to suspend, add 500g of treated HPD-300 macroporous adsorption resin to the chromatography column, and absorb after loading 1 hour, eluted with 2500ml of water, then eluted with 3000ml of ethanol with a volume concentration of 20% and 4000ml of ethanol with a volume concentration of 60%, and collected the ethanol elution solution with a volume concentration of 60%, concentrated under reduced pressure, and dried in vacuo 28.9 g of the crude extract powder was obtained, and the extraction yield was 4.82%.

[0032] 3. Separation and purification of monomeric compounds:

[0033...

Embodiment 2

[0044] 1. Medicinal material extraction: Weigh 600 g of kiwi fruit leaves, reflux extraction with 6 times volume concentration of 60% ethanol twice, each time for 2 hours, filter, combine filtrates, concentrate under reduced pressure at 50 ° C until no alcohol smell, to obtain Concentrated extract.

[0045] 2. Preparation of the crude extract: Take 1000ml of the concentrated extract, add an equal amount of water to suspend it, add 500g of treated DM-301 macroporous adsorption resin to the chromatographic column, after loading the sample Adsorbed for 1 hour, eluted with 2500ml of water, and then eluted with 3000ml of ethanol with a volume concentration of 20% and 4000ml of ethanol with a volume concentration of 60%, and collected the ethanol eluting solution with a volume concentration of 60%, concentrated under reduced pressure, and vacuumed After drying, 27.5 g of the crude extract powder was obtained, and the extraction yield was 4.58%.

[0046] 3. The methods and steps of ...

Embodiment 3

[0048] 1. Medicinal material extraction: Weigh 600 g of kiwifruit leaves, reflux extraction with 6 times the volume concentration of 65% ethanol twice, each time for 2 hours, filter, combine the filtrates, concentrate under reduced pressure at 50 ° C until there is no alcohol smell, and obtain Concentrate the extract.

[0049] 2. Preparation of the crude extract: Take 1000ml of the concentrated extract, add an equal amount of water to suspend, add 500g of treated HPD-300 macroporous adsorption resin to the chromatography column, after the sample is loaded Adsorbed for 1 hour, eluted with 3000ml of water, then eluted with 3000ml of ethanol with a volume concentration of 20% and 4500ml of ethanol with a volume concentration of 50%, and collected the ethanol elution solution with a volume concentration of 60%, concentrated under reduced pressure, and vacuumed Dry to obtain 30.2 g of crude extract powder, and the extraction yield is 5.03%.

[0050] 3. The methods and steps of sep...

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Abstract

The present invention discloses a method for separating and preparing high purity flavonoid glycoside compounds from actinidia valvata dunn leaves. The method comprises processes of drug material extraction, crude extract preparation, and monomer compound separation and purification. The drug material extraction process, actinidia valvata dunn leaves are subjected to reflux extraction 2-4 times with ethanol with a volume concentration of 50-80%, and then the ethanol is subjected to vacuum recovering to obtain the extracting solution. In the crude extract preparation process, the extracting solution is loaded on a macroporous adsorption resin, water, ethanol with a volume concentration of 20-30%, and ethanol with a volume concentration of 50-60% are respectively adopted to carry out elution treatments, the eluent after elution with the ethanol with the volume concentration of 50-60% is collected, and is concentrated and dried to obtain the crude extract. In the monomer compound separation and purification process, a high-speed counter-current chromatography method is adopted to separate and purify the resulting crude extract, wherein the concrete steps comprise: preparing a solvent system for forming a stationary phase and a mobile phase, filling the stationary phase in a counter-current chromatography column, rotating the column, pumping the mobile phase into the column, adding the prepared crude extract to an injection valve, and receiving the target flow part according to a detection map.

Description

technical field [0001] The present invention relates to a flavonoid glycoside compound prepared from the leaves of kiwifruit opposite calyx, that is, kaempferol-3-O-α-L-rhamnosyl-(1→3)-α-L-rhamnosyl- (1→6)-β-D-galactopyranoside, kaempferol-3-O-α-L-rhamnosyl-(1→3)-(4-O-acetyl-α-L -rhamnosyl)-(1→6)-β-D-galactopyranoside and kaempferol-3-O-α-L-rhamnosyl-(1→3)-(2,4 - a process for di-O-acetyl-α-L-rhamnosyl)-(1→6)-β-D-galactopyranoside. Background technique [0002] Actinidia valvata Dunn is a plant of Actinidia genus Actinidia, mainly distributed in Anhui, Zhejiang, Jiangxi and other East China regions. Its root is cat ginseng, which is a commonly used anti-tumor traditional Chinese medicine in East China. In recent years, inventors have put a lot of energy into a series of pharmaceutical research on this medicinal plant [H.L.Xin, Y.C.Wu, Y.F.Xu, et al.Chin J Nat Med., 2010, 8: 260; H.L.Xin, X.Q.Yue, Y.F. Xu, et al.Helv.Chim.Acta, 2008, 91:575; Y.F Xu, R.L.Ge, J.Du, et al.Can...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/07
Inventor 辛海量凌昌全曲丽萍苏永华郑国银李同明彭浩
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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