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Method for preparing high-purity quercetagetin

A high-purity quercetin-tagoldin technology, applied in organic chemistry and other fields, can solve problems such as high production cost, low recovery rate, and complicated steps, and achieve the effects of low sample loss, high recovery rate, and large separation volume

Active Publication Date: 2013-03-13
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the methods of purifying flavonoids are mainly macroporous resin purification or column chromatography. The macroporous resin purification method has complicated steps and low recovery rate, while column chromatography requires a large amount of chromatography packing material, and it needs to be replaced and cleaned frequently during the production process. , Activation of fillers, not only makes the production cost high, but also has a large workload and low recovery rate

Method used

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  • Method for preparing high-purity quercetagetin
  • Method for preparing high-purity quercetagetin

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Experimental program
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Effect test

Embodiment 1

[0022] It is separated by a high-speed countercurrent chromatographic system with a column volume of 300ml (equipped with TBP-5002 constant current and constant pressure pump, HD-3 ultraviolet detector), and chloroform, n-butanol and water are selected as the solvent system, according to the volume ratio of 4:3:3 Put the above solvent components in a separatory funnel, shake well and let stand to separate layers. After equilibrating for a certain period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase).

[0023] Put 30 g of fermented marigold lutein lipid extraction residue in 300 mL of 5% ethanol aqueous solution, extract at 30° C. for 10 h, and filter to obtain a crude quercetin tagetin extract. Concentrate 30 g of the quercetin-tagerin crude extract to a paste under reduced pressure, dissolve it in 30 ml of mobile phase, and obtain a solution containing quercetin-tagenate for use. Use the solution containing quercetin tagetin as the in...

Embodiment 2

[0025] A high-speed countercurrent chromatography system with a column volume of 1000ml was used for separation. Select n-hexane, ethanol and water as the solvent system, put the above-mentioned solvent components in a separatory funnel according to the volume ratio of 5:2:3, shake well and let stand to separate layers. After equilibrating for a certain period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase).

[0026] Place 150 g of the fermented marigold lutein extract residue in 1500 mL of 50% ethanol aqueous solution, extract at 60° C. for 6 h, and filter to obtain a crude quercetin tagetin extract. Concentrate 100 g of the quercetin-tagerin crude extract under reduced pressure to a paste, dissolve it in 150 ml of mobile phase, and obtain a solution containing quercetin-tagenate for use. Use the solution containing quercetin tagetin as the injection sample. Before the injection, fill the entire column with the stationary phase, adjust...

Embodiment 3

[0028] A high-speed countercurrent chromatographic system with a column volume of 5000ml was used for separation. Ethyl acetate, methanol and water were selected as the solvent system, and the above solvent components were placed in a separatory funnel according to the volume ratio of 1:1:1, shaken evenly, and allowed to stand and separate into layers. After equilibrating for a certain period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase).

[0029] Put 300 g of fermented marigold lutein extract residue in 3000 mL of 90% ethanol aqueous solution, extract at 90° C. for 0.5 h, and filter to obtain a crude quercetin tagetin extract. Concentrate 300g of quercetin-tagetine crude extract under reduced pressure to a paste, dissolve it in 300ml of mobile phase, and obtain a solution containing quercetin-tagagene for use. Use the solution containing quercetin tagetin as the injection sample. Before the injection, fill the entire column with the ...

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Abstract

The invention discloses a method for preparing high-purity quercetagetin and belongs to the technical field of flavonoids compound extraction. The method comprises the following steps of: extracting fermented residue subjected to marigold flower lutein ester extraction by using 5 to 90 percent aqueous solution of ethanol to obtain a crude extract of quercetagetin, concentrating under reduced pressure to obtain a paste, and dissolving in a mobile phase to obtain solution containing the quercetagetin; separating and purifying the quercetagetin from the solution containing the quercetagetin by adopting a preparative high-speed countercurrent chromatograph; and performing high performance liquid chromatography (HPLC) detection, wherein the product with the purity of over 95 percent is qualified. The method has the advantages of low requirement on solvent purity, large separation amount, low loss of samples, high recovery rate and the like, and is suitable for separating and preparing the quercetagetin on various scales from laboratory preparation to industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction of flavonoids, and in particular relates to a preparation method of high-purity quercetin-tagetine. Background technique [0002] Marigold is widely planted all over the world. In addition to its ornamental value, it also has good medicinal value. Its functional components mainly include carotenoids, flavonoids, terpenoids and essential oils. Quercetin tagetin is a unique flavonoid compound of marigold, its characteristics are mainly manifested in: it has the antioxidant activity of scavenging free radicals, and its antioxidant effect is mainly manifested in its ability to scavenge singlet oxygen and oxygen-containing free radicals , in the anti-oxidation reaction, it can not only remove the free radicals in the chain initiation stage, but also directly capture the free radicals in the free radical reaction chain and block the free radical chain reaction; marigold has strong anti-tumor, anti-ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/30
Inventor 高彦祥闫秋丽刘璇袁芳侯占群
Owner CHINA AGRI UNIV
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