Preparation method for fast separating flavonoid glycosides from oil-tea-cakes with medium pressure column

A technology of flavonoid glycosides and oil tea cakes in meal, which is applied in the field of preparation of flavonoid glycosides, and can solve the problems of slow separation process and low yield of silica gel column chromatography

Active Publication Date: 2010-12-01
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] It has been reported in domestic literature that Yu Bin et al. used silica gel column chromatography to separate two main flavonoid glycosides from camellia oleifera dry cake, and established its liquid chromatography analysis method. However, the separation process of ordinary silica gel co

Method used

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  • Preparation method for fast separating flavonoid glycosides from oil-tea-cakes with medium pressure column
  • Preparation method for fast separating flavonoid glycosides from oil-tea-cakes with medium pressure column
  • Preparation method for fast separating flavonoid glycosides from oil-tea-cakes with medium pressure column

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Experimental program
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Effect test

Embodiment 1

[0030] Step one, degreasing:

[0031] Camellia oleifera seeds were shelled, seeds were crushed, and petroleum ether was used to degrease, the ratio of tea seeds to petroleum ether was 1:30g / mL, the temperature was 60°C, extraction was carried out for 2 hours, extracted 3 times, and the filter residue was obtained after filtration to obtain defatted camellia oleifera seed meal;

[0032] The second step, extract:

[0033] Add 1 g of raw material to 20 mL of 70% concentration alcohol-water solution to extract 3 times, extraction temperature is 80°C, extraction time is 2 hours, after extraction, filter, combine filtrates, concentrate in vacuum to obtain crude extract of flavonoid glycosides of camellia oleifera;

[0034] The third step, extraction:

[0035] The extract obtained from the extract is extracted 4 times with n-butanol, and the aqueous layer is concentrated to obtain a phase extract;

[0036] The fourth step, medium pressure column purification:

[0037] The crude ex...

Embodiment 2

[0044] Step one, degreasing:

[0045] Camellia oleifera seeds were shelled, seeds were crushed, and petroleum ether was used to degrease, the ratio of tea seeds to petroleum ether was 1:30g / mL, the temperature was 60°C, extraction was carried out for 2 hours, extracted 3 times, and the filter residue was obtained after filtration to obtain defatted camellia oleifera seed meal;

[0046] The second step, extract:

[0047] Add 1 g of raw material to 20 mL of 50% methanol solution for extraction of Camellia oleifera seed meal for 3 times, extraction temperature is 80°C, extraction time is 2 hours, after extraction, filter, combine the filtrates, and vacuum concentrate to obtain the crude extract of flavonoid glycosides of camellia oleifera meal;

[0048] The third step, extraction:

[0049] The extract obtained from the extract is extracted 4 times with acetone, and the aqueous layer is concentrated to obtain a crude extract;

[0050] The fourth step, medium pressure column puri...

Embodiment 3

[0055] Step one, degreasing:

[0056] Camellia oleifera seeds were shelled, seeds were crushed, and petroleum ether was used to degrease, the ratio of tea seeds to petroleum ether was 1:30g / mL, the temperature was 60°C, extraction was carried out for 2 hours, extracted 3 times, and the filter residue was obtained after filtration to obtain defatted camellia oleifera seed meal;

[0057] The second step, extract:

[0058] Add 1 g of raw material to 20 mL of 70% ethanol solution to extract 3 times of Camellia oleifera seed meal, extraction temperature is 80°C, extraction time is 2 hours, after extraction, filter, combine filtrate, vacuum concentrate to obtain crude extract of flavonoid glycosides of camellia oleifera meal;

[0059] The third step, extraction:

[0060] The extract obtained from the extract was extracted 4 times with n-butanol, and the aqueous layer was concentrated to obtain a crude extract;

[0061] The fourth step, medium pressure column purification:

[0062...

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Abstract

The invention discloses a preparation method for fast separating flavonoid glycosides from oil-tea-cakes with a medium pressure column, which comprises the following steps of: decorticating and crushing camellia oleifera abel seeds, degreasing the camellia oleifera abel seeds with non-polar solvents, performing extraction with ethanol water, filtering and condensing the extract to obtain crude extract concrete, performing fast separation with the medium pressure column to obtain an over 90 percent flavonoid glycoside mixture, and further adopting a high performance liquid chromatography to prepare over 95 percent flavonoid glycoside monomers, wherein the flavonoid glycoside monomers are kaemplerol 3-O-[2-O-beta-D-galactose-6-O-alpha-L-rhamnose]-beta-D-glucoside (I) and kaemplerol 3-O-[2-O-beta-D-xylose-6-O-alpha-L-rhamnose]-beta-D-glucoside (II) respectively. The method can be used for batch preparation, and has the advantage of providing quality raw materials for the development of flavonoid glycoside medicaments and healthcare functional products in the oil-tea-cakes.

Description

technical field [0001] The invention relates to the technical field of plant extracts, in particular to a medium-pressure rapid separation method for preparing flavonoid glycosides from camellia oleifera cake. Background technique [0002] Camellia oleifera (Camellia oleifera Abel.), also known as tea seed tree, camellia oleifera, and white flower tea, belongs to the plant of the genus Camellia in the family Theaceae. It is a perennial tree or shrub with more than 100 varieties. Camellia oleifera is a unique woody oil plant in my country. It has a cultivation history of more than 2,000 years in China and is now mainly distributed in more than 1,100 counties in 14 provinces in the Huaihe River and Yangtze River basins and south of my country. my country produces only 200,000 tons of crude tea oil per year, while the remaining tea seed meal after oil extraction is about 500,000 tons per year. Camellia oleifera cake after oil extraction contains protein, crude fiber, carbohydr...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/07
Inventor 王成章陈虹霞叶建中周昊原姣姣
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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