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Extraction separation method for isorhamnetin-3-O-beta-D-rutinoside in caragana sinica flower bud

A separation method, gorse technology, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of difficult scale-up production, high gel market price, small processing capacity, etc., and the method is simple Feasible, less loss, easy regeneration effect

Inactive Publication Date: 2014-11-05
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, there are few reports on the extraction method of isorhamnetin-3-O-β-D-rutinose. Isorhamnetin-3-O-β-D-rutinoside with a purity of more than 98% was isolated from the total flavonoids in Jibuza leaves by Sephadex LH-20 gel column The reference substance, the method is simple and effective, but the gel material is used for purification in the key step of the method, and the gel has the problems of high market price and small processing volume, which leads to isorhamnetin-3-O-β-D-rutinose is low, and it is not easy to expand the production

Method used

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  • Extraction separation method for isorhamnetin-3-O-beta-D-rutinoside in caragana sinica flower bud
  • Extraction separation method for isorhamnetin-3-O-beta-D-rutinoside in caragana sinica flower bud
  • Extraction separation method for isorhamnetin-3-O-beta-D-rutinoside in caragana sinica flower bud

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: Isorhamnetin-3-O- in this gorse flower bud β -The extraction and separation method of D-rutinose, the specific content is as follows:

[0029] (1) Crushing and extraction

[0030] Take 10 kg of gorse flower buds dried in the shade, crush them (the diameter of the fragments is about 1.5 mm), add 12 times the mass percentage of ethanol water solution with a concentration of 75%, reflux extraction twice, each time for 1.5 hours, and extract the extract while it is hot. , to obtain a crude sample of 1.5 kg of the extract;

[0031] (2) Extraction, separation and purification

[0032] Add 3 times the weight of the crude extract to the crude extract to dissolve in hot water at 45°C. The solution is first extracted three times with petroleum ether, and the petroleum ether extraction phase is discarded, then extracted three times with ethyl acetate, and the ethyl acetate extraction phase is discarded. , and finally extracted three times with n-butanol, the combi...

Embodiment 2

[0047] Embodiment 2: Isorhamnetin-3-O- in this gorse flower bud β -The extraction and separation method of D-rutinose, the specific content is as follows:

[0048] (1) Crushing and extraction

[0049] Take 10 kg of gorse flower buds dried in the shade, crush them (the diameter of the fragments is about 1.0 mm), add 15 times the mass percentage of ethanol water solution with a concentration of 70%, reflux extraction twice, each time for 1.0 hours, extract and concentrate while hot , to obtain a crude sample of 1.8 kg of extract;

[0050] (2) Extraction, separation and purification

[0051] Add 4 times the weight of the crude extract to the crude extract to dissolve in hot water at 40°C. The solution is first extracted twice with petroleum ether, discard the petroleum ether extract, then extract twice with ethyl acetate, and discard the ethyl acetate. The extract phase was finally extracted 3 times with n-butanol, and the n-butanol extracts were combined and concentrated to ...

Embodiment 3

[0052] Embodiment 3: Isorhamnetin-3-O- in the flower buds of this gorse β -The extraction and separation method of D-rutinose, the specific content is as follows:

[0053] (1) Crushing and extraction

[0054] Take 10 kg of shade-dried gorse flower buds, crush them (the diameter of the fragments is about 2mm), add 15 times the mass percentage of ethanol water solution with a concentration of 80%, and reflux twice for 1.2 hours each time. The extract is extracted and concentrated while it is hot. 2.1kg crude extract sample was obtained;

[0055] (2) Extraction, separation and purification

[0056] Add 5 times the weight of the crude sample to the crude extract to dissolve in hot water at 50°C. The solution is first extracted three times with petroleum ether, and the petroleum ether extraction phase is discarded, then extracted three times with ethyl acetate, and the ethyl acetate is discarded. Finally, it was extracted with n-butanol for 3 times, and the n-butanol extracts w...

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Abstract

The invention discloses an extraction separation method for isorhamnetin-3-O-beta-D-rutinoside in caragana sinica flower bud. The method comprises: performing crushing, refluxing extraction and concentration on dry caragana sinica flower buds, so as to obtain a crude extractive; firstly performing extraction segmentation on the crude extractive, selecting solvent systems petroleum ether, ethyl acetate and n-butanol, performing separation elution on the n-butanol-containing extraction part through polyamide phenol resin, concentrating the eluate until no alcohol smell exists, cooling, standing, and filtering to obtain isorhamnetin-3-O-beta-D-rutinoside. The content of isorhamnetin-3-O-beta-D-rutinoside prepared by employing the method is larger than 80%. The method is high in extraction rate, low in equipment requirement and easy for expanded production, and is suitable of industrialized production.

Description

technical field [0001] The invention relates to the field of deep processing of natural resources, more specifically to a method of extracting and separating rhamnin-3-O- β -D-Rutinose method. Background technique [0002] broom( Caragana sinica ) for the Fabaceae Caragana ( Caragana ) deciduous shrubs, alias Caragana, yellow bird, sun bird, blood grass. Gorse is distributed in the Yangtze River Basin of my country and the hills and mountainous sunny slopes of North China. There are more than 40 species produced in China, and the resources are relatively abundant. In Yunnan, winter ends and spring comes, and gorse blooms all over the mountains and fields. Its appearance is not outstanding, but its fragrance is unique. People stir-fry it with eggs, bacon, ham and fresh meat, or cook it with sliced ​​meat and tofu to make a three-flavored soup, which is sweet and delicious. A folk proverb says: "If you eat gorse, your eyes will not blink." Zhang Xiaoling et al. (2004) ...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 太志刚陈安逸蔡乐秦本逵
Owner KUNMING UNIV OF SCI & TECH
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