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Method for separating and purifying flavonoid compounds in polygonum multiflorum leaf ethyl acetate phase through high-speed counter-current chromatography

A technology of high-speed countercurrent chromatography and flavonoids, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of large solvent consumption, poor separation effect, and large sample loss, and achieve low overall cost , small sample loss, simple operation

Active Publication Date: 2021-09-17
INST OF APPLIED CHEM JIANGXI ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing separation technology, traditional column chromatography separation, recrystallization and other methods are generally used to extract and separate monomeric compounds from Polygonum multiflorum samples. These methods need repeated column chromatography separation, complicated operation and long time consumption. Not only the solvent consumption is large, Moreover, the sample loss is also large, and the separation effect is poor.

Method used

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  • Method for separating and purifying flavonoid compounds in polygonum multiflorum leaf ethyl acetate phase through high-speed counter-current chromatography
  • Method for separating and purifying flavonoid compounds in polygonum multiflorum leaf ethyl acetate phase through high-speed counter-current chromatography
  • Method for separating and purifying flavonoid compounds in polygonum multiflorum leaf ethyl acetate phase through high-speed counter-current chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step 1: Preparation of Ethyl Acetate Phase of Radix Polygoni Multiflori

[0032] 1.0 kg of dried Polygonum multiflorum leaves were subjected to ultrasonic extraction with 90% ethanol as a solvent, the extraction time was 2 hours, and the solid-to-liquid ratio of ultrasonic extraction was 1:15, filtered, and the filter residue was treated twice; the filtrates were combined and subjected to vacuum Concentrate under reduced pressure until there is no ethanol smell to obtain the ethanol extract of Polygonum multiflorum leaves, and then add ethyl acetate and water for multiple extractions. The ethyl acetate phase after complete extraction was concentrated under reduced pressure in vacuo to remove the solvent to obtain the ethyl acetate phase of Radix Polygoni Multiflori.

[0033] Step 2: Separation of flavonoid monomers

[0034] Use water-methanol-ethyl acetate-n-hexane with a volume ratio of 2:1:3:0.5 as the solvent system, shake well and let stand, separate the upper and ...

Embodiment 2

[0040] Step 1: Preparation of Ethyl Acetate Phase of Radix Polygoni Multiflori

[0041] 1.0 kg of dried Polygonum multiflorum leaves were subjected to ultrasonic extraction with 85% ethanol as a solvent, the extraction time was 1 h, and the solid-to-liquid ratio of ultrasonic extraction was 1:20, filtered, and the filter residue was treated once again; the filtrates were combined and subjected to vacuum Concentrate under reduced pressure until there is no ethanol smell to obtain the ethanol extract of Polygonum multiflorum leaves, and then add ethyl acetate and water for multiple extractions. The ethyl acetate phase after complete extraction was concentrated under reduced pressure in vacuo to remove the solvent to obtain the ethyl acetate phase of Radix Polygoni Multiflori.

[0042] Step 2: Separation of flavonoid monomers

[0043] Use water-methanol-ethyl acetate-n-hexane with a volume ratio of 2:2:4:0.5 as the solvent system, shake well and let stand, separate the upper and...

Embodiment 3

[0047] Step 1: Preparation of Ethyl Acetate Phase of Radix Polygoni Multiflori

[0048] 1.0 kg of dried Polygonum multiflorum leaves were subjected to ultrasonic extraction with 95% ethanol as a solvent, the extraction time was 3 hours, the solid-to-liquid ratio of ultrasonic extraction was 1:10, filtered, and the filter residue was treated twice; the filtrates were combined and subjected to vacuum Concentrate under reduced pressure until there is no ethanol smell to obtain the ethanol extract of Polygonum multiflorum leaves, and then add ethyl acetate and water for multiple extractions. The ethyl acetate phase after complete extraction was concentrated under reduced pressure in vacuo to remove the solvent to obtain the ethyl acetate phase of Radix Polygoni Multiflori.

[0049] Step 2: Separation of flavonoid monomers

[0050] Use water-methanol-ethyl acetate-n-hexane with a volume ratio of 2:1:4:1 as the solvent system, shake well and let stand, separate the upper and lower ...

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Abstract

The invention relates to a method for separating and purifying flavonoid compounds in polygonum multiflorum leaves through high-speed counter-current chromatography, which comprises the following steps: (1) preparing an ethyl acetate phase of the polygonum multiflorum leaves, (2) adopting a water-methanol-ethyl acetate-normal hexane solution with the volume ratio of 1: 1: 1: 0.5-2: 2: 5: 1 as a solvent system, and pumping a stationary phase and a mobile phase into a high-speed counter-current chromatograph; when the two-phase solvent system is balanced in the high-speed counter-current column, dissolving the polygonum multiflorum leaf ethyl acetate phase in the two-phase solvent system, and carrying out high-speed counter-current chromatographic separation; during high-speed countercurrent chromatography separation, an ultraviolet detector detecting a wave peak, performing collection from peak appearance until the peak disappears, collecting different fractions respectively, and performing vacuum concentration and freeze drying to obtain myricetin, quercitrin and kaempferol-3-O-rhamnoside. The separated and purified flavonoid compound monomer is high in purity, small in loss, easy to operate, large in preparation amount, economical and environmentally friendly.

Description

technical field [0001] The invention relates to the field of natural product chemistry, in particular to a method for separating and purifying flavonoids in the ethyl acetate phase of Polygonum multiflorum leaves by high-speed countercurrent chromatography. Background technique [0002] Polygonum multiflorum Thunb., also known as Yejiaoteng, Shouwuteng, is the dry tuber of the perennial herb Polygonum multiflorum (Fallopia Adans.) in the family Polygonaceae. It is recorded in "Compendium of Materia Medica" and "Chinese Pharmacopoeia". "Compendium of Materia Medica" says "sweet in nature, flat; heart-guiding, liver meridian. It has the effects of nourishing blood and calming the nerves, dispelling wind and dredging collaterals. It is used for insomnia, dreaminess, Blood deficiency body pain, rheumatic arthralgia, skin itching and other diseases." Studies have shown that Polygonum multiflorum contains a variety of biologically active substances, the most important of which inc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
CPCC07H17/07C07H1/08
Inventor 吴磊吴静谢传奇徐敢珍熊伟曹明源
Owner INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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