Method for preparing myricetin by using vine tea and application of pyrosulfite

A technology of metabisulfite and rattan tea, applied in the direction of organic chemistry and the like, can solve the problems of difficult industrialized production, low yield of myricetin extraction and preparation, and achieve high yield, extensive industrial production, and low equipment requirements.

Inactive Publication Date: 2013-09-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention is aimed at the lack of myricetin resources, the extraction and preparation yield of myricetin in the prior art is low, up to 8%, and it is difficult to deal with the problem ...

Method used

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  • Method for preparing myricetin by using vine tea and application of pyrosulfite
  • Method for preparing myricetin by using vine tea and application of pyrosulfite
  • Method for preparing myricetin by using vine tea and application of pyrosulfite

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Experimental program
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Embodiment 1

[0031] 1. Extraction of rattan tea

[0032] Weigh 20g of dried rattan tea powder, add about 200mL of water, heat to 95°C to extract for 1 hour, filter while hot, repeat the above operation twice for the filter residue, combine the filtrate three times, concentrate to 200mL, and then stand at 0-5°C for precipitation Pale yellow precipitate, filter with suction, dissolve the filter precipitate with 300mL of absolute ethanol, let it sit for suction filtration, concentrate the filtrate to 100mL under reduced pressure, and obtain the ethanol extract of the extract, which is set aside;

[0033] 2. Dehydrogenation reaction of dihydromyricetin

[0034] Add 100 mL of the concentrated extract above to 250 mL of 20% Na 2 S 2 o 5 In an aqueous solution, react at 100°C for 4 hours; to complete the reaction, pour the mixed solution into an ice-water mixture, let it stand still to precipitate a precipitate, filter with suction, wash the precipitate with ice water several times, and then d...

Embodiment 2

[0037] 1. Extraction of vine tea:

[0038] Weigh 20g of dried vine tea powder, add 200mL of water, heat to 95°C for extraction for 1 hour, filter while hot, repeat the above operation twice for the filter residue, combine the filtrate three times, concentrate to 200mL; Suction filter the yellow precipitate, dissolve the filtered precipitate with 300mL of absolute ethanol, let it stand for suction filtration, and concentrate the filtrate to 100mL under reduced pressure to obtain the ethanol extract of the extract, which is set aside.

[0039] 2. Dehydrogenation reaction of dihydromyricetin:

[0040] Add 100 mL of the concentrated extract above to 250 mL of 20% K 2 S 2 o5 In an aqueous solution, react at 100°C for 4 hours; to end the reaction, pour the mixed solution into an ice-water mixture, let it stand still to precipitate a precipitate, filter with suction, wash the precipitate with ice water several times, and then dry it in a vacuum at 40°C to obtain a yellow-green soli...

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Abstract

The invention discloses a method for preparing myricetin by using vine tea and an application of pyrosulfite. The method comprises the following steps of: extracting the ground vine tea with hot water, filtering while the vine tea is hot, concentrating the filter liquor and cooling to separate out sediments; carrying out suction filtration, dissolving the sediment residue with absolute ethyl alcohol, filtering to remove undissolved substances, and concentrating the ethanol solution obtained from filtration to obtain ethyl alcohol extract; adding the ethyl alcohol extract into the pyrosulfite solution for reaction, then pouring the reaction liquid into an ice-water mixture, and crystallizing, filtering, washing and drying to obtain the myricetin. According to the application, the pyrosulfite is applied to the vine tea as a dehydrogenation oxidizing agent for dehydrogenation transformation from dihydromyricetin to myricetin, and the transformation efficiency is high. By using the method, materials are low in cost and can be easily obtained. The method is simple, pollution-free and low in equipment requirement and can be widely applied to industrial production. The yield of the prepared myricetin reaches 21% in comparison with materials, and the purity reaches 96%.

Description

Technical field: [0001] The invention relates to a method for preparing myricetin from vine tea and the application of pyrosulfite, belonging to the field of extraction and enrichment preparation of active ingredients of natural products. Background technique [0002] All plants of the genus Vitis vinifera contain flavonoid components myricetin and dihydromyricetin, among which the content of Snake-toothed grape is the highest, and the processed products of Snake-toothed grape stems and leaves are commonly known as vine tea, which is rich in various Active ingredients, such as dihydromyricetin, myricetin, catechin, gallic acid, amino acids, polysaccharides, etc., of which the content of dihydromyricetin is the highest, and myricetin is low. According to the existing literature and patent reports, most studies focus on the extraction and purification of dihydromyricetin, which is high in vine tea, but there are few studies on myricetin. The relevant patent documents include: ...

Claims

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Application Information

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IPC IPC(8): C07D311/30
Inventor 钟世安孔艳月张春静李翠娥周玲李晓静
Owner CENT SOUTH UNIV
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