Extraction and Separation of Rhamnetin-3-o-β-d-Rutinose from Gorse Flower Buds

A separation method and gorse technology, which are applied in chemical instruments and methods, sugar derivatives, sugar derivatives and other directions, can solve the problems of difficult to scale up production, high market price, small processing capacity, etc., and achieve the method is simple and feasible, The effect of reducing the amount of loss and easy regeneration

Inactive Publication Date: 2016-06-22
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, and so far only Li Kunping et al. (2011) used macroporous adsorption resin to enrich the total For flavonoids, use SephadexLH-20 gel column to separate and prepare isorhamnetin-3-O-β-D-rutinoside reference substance with a purity greater than 98% from total flavonoids. The method is simple and effective, but the key step of the method uses gel Gel materials are purified, but the gel has the problems of high market price and small processing volume, which leads to low yield of isorhamnetin-3-O-β-D-rutinose and is not easy to expand production

Method used

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  • Extraction and Separation of Rhamnetin-3-o-β-d-Rutinose from Gorse Flower Buds
  • Extraction and Separation of Rhamnetin-3-o-β-d-Rutinose from Gorse Flower Buds
  • Extraction and Separation of Rhamnetin-3-o-β-d-Rutinose from Gorse Flower Buds

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: The extraction and separation method of isorhamnetin-3-O-β-D-rutinose in the gorse flower buds, the specific contents are as follows:

[0029] (1) Crushing and extraction

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

[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 combined...

Embodiment 2

[0047] Embodiment 2: The extraction and separation method of isorhamnetin-3-O-β-D-rutinose in the gorse flower buds, the specific contents are as follows:

[0048] (1) Crushing and extraction

[0049] Take 10kg of shade-dried gorse flower buds, crush them (the diameter of the fragments is about 1.0mm), add 15 times the mass percentage of ethanol aqueous solution with a concentration of 70%, and reflux twice for 1.0 hours each time. The extract is extracted and concentrated while it is hot. The crude sample of the extract was 1.8kg;

[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 t...

Embodiment 3

[0052] Embodiment 3: The extraction and separation method of isorhamnetin-3-O-β-D-rutinose in the gorse flower buds, the specific contents are as follows:

[0053] (1) Crushing and extraction

[0054] Take 10kg of gorse flower buds dried in the shade, crush them (the diameter of the fragments is about 2mm), add 15 times the mass percentage concentration of 80% ethanol aqueous solution, reflux extraction twice, each time for 1.2 hours, extract while hot and concentrate, to obtain Extract crude sample 2.1kg;

[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 were combined and concentrated t...

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Abstract

The invention discloses isorhamnetin-3-O- β - The extraction and separation method of D-rutin, the dried gorse flower buds are crushed, refluxed, extracted, and concentrated to obtain a crude sample of the extract; the crude sample of the extract is first extracted and sectioned, and the solvent system is petroleum ether and ethyl acetate And n-butanol, the extracted part containing n-butanol is further separated and eluted by polyamide phenol resin column, the eluate is concentrated until it has no alcohol smell, the pH is adjusted to 2~3, cooled and stood, and filtered to obtain isorhamnetin-3 -O- β -D-rutinose; the isorhamnetin-3-O- that the inventive method makes β -D-rutinose content > 80%, the method has a high extraction rate, low equipment requirements, easy to expand production, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of deep processing of natural resources, in particular to a method for extracting and separating rhamnin-3-O-β-D-rutinose from gorse flower buds. Background technique [0002] Caraganasinica (Caraganasinica) is a deciduous shrub of the genus Caragana of the Fabaceae family. Gorse is distributed in the Yangtze River Basin of China 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) and Fan Jian et al. (2006) report...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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