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Method for preparing tea tree purple bud anthocyanin high-purity products through separation

An anthocyanin and purple bud technology, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems such as failure to make breakthrough progress and low content, and achieve low production cost and high yield. , the effect of simple production process

Inactive Publication Date: 2018-09-04
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with blackberry, cranberry, red raspberry, purple potato and other plant resources, anthocyanins in tea have lower content and more types, so that in the separation and preparation of high-purity tea anthocyanins or monomers, it has not been possible to obtain breakthrough

Method used

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  • Method for preparing tea tree purple bud anthocyanin high-purity products through separation
  • Method for preparing tea tree purple bud anthocyanin high-purity products through separation
  • Method for preparing tea tree purple bud anthocyanin high-purity products through separation

Examples

Experimental program
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Effect test

Embodiment 1

[0031] With one bud and two leaves of Zijuan tea tree as raw material, vacuum freeze-dry the tea leaves, grind them into powder, add 70% volume concentration ethanol solution containing 5% glacial acetic acid, stand at room temperature and avoid light for 3 (solid-liquid ratio is 1g:25ml, and each extraction time is 24h), obtains extract; Prepare n-hexane by volume ratio: ethyl acetate: the mixed solvent of water=1:1:1.5, use this mixed solvent to The extract is extracted and degreased; put the degreased extract on a sodium-type 732 cation exchange resin column, first adopt 90% volume concentration of ethanol solution to elute to remove polyphenol impurities, and then use 4% HCI-ethanol solution to carry out gradient washing (The ethanol volume concentration of gradient elution is 50%, 60%, 70%, 80%, 90%), collect the eluate according to the concentration gradient, combine the eluate, and concentrate at -0.05MPa, 45°C to remove The organic phase was passed through D101 macropo...

Embodiment 2

[0033] Using purple bud tea tree optional 9803 with one bud and two leaves as raw material, the tea leaves are vacuum freeze-dried, ground into powder, and extracted with 80% ethanol solution containing 1% glacial acetic acid at room temperature and protected from light 3 times (the ratio of solid to liquid is 1g:22ml, and the extraction time is 20h each time), the extract is obtained; prepare n-hexane by volume ratio: ethyl acetate: a mixed solvent of water=1.2:1.2:1.8, and use the mixed solvent Extract and degrease the extract; put the degreased extract on a sodium-type 732 cation exchange resin column, first use 90% ethanol solution to elute to remove polyphenol impurities; then use 4% HCI-ethanol solution for gradient elution (The ethanol volume concentration of gradient elution is 50%, 60%, 70%, 80%, 90%), respectively collect eluate according to concentration gradient, combine eluate, concentrate at -0.07MPa, 42 ℃ to remove organic matter Phase, pass through D101 macropo...

Embodiment 3

[0035] Using purple bud tea tree, red bud bergamot, one bud and two leaves as raw materials, vacuum freeze-dry the tea leaves, grind them into powder, add 90% volume concentration of ethanol solution containing 10% volume fraction of glacial acetic acid, stand at room temperature and avoid light for extraction 2 times (the ratio of solid to liquid is 1g:25ml, and the extraction time is 12h each time), the extract is obtained; prepare n-hexane by volume ratio: ethyl acetate: water=1.5:1.5:2 mixed solvent, with the mixed solvent Extract and degrease the extract; put the degreased extract on a sodium-type 732 cation exchange resin column, first use ethanol solution with a volume concentration of 90% to remove polyphenol impurities; then use 4% HCI-ethanol solution for gradient Elution (volume concentration of ethanol for gradient elution is 50%, 60%, 70%, 80%, 90%), collect the eluate according to the concentration gradient, combine the eluate, concentrate at -0.07MPa, 38°C Remov...

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Abstract

The invention provides a method for preparing tea tree purple bud anthocyanin high-purity products through separation. The method comprises the following steps: extracting tea tree purple buds by an acidic ethanol solution, performing extraction to defat, performing strong acid type action exchange resin separation to remove impurities, performing high-speed countercurrent chromatographic separation to obtain anthocyanin refined products, and performing purification by preparation type high performance liquid chromatography to obtain five anthocyanin high-purity products. According to the method, the fresh leaves of the purple bud tea tree varieties (Zijuan, red bud fingered citron, An 73 and optional 9803) rich in anthocyanin as raw materials and multi-stage separation and purification process technologies are creatively applied; meanwhile, the five tea tree purple bud anthocyanin high-purity products with single anthocyanin purity being more than 90 percent are prepared, wherein thepurity of delphinidin-3-O-(6-(E)p-coumaric acid)pyran galactoside exceeds 98 percent and the monomer quality requirement is met. The whole production process is simple, low in production cost and highin operability; high-quality raw materials are provided for research on pharmacology and medical efficacy and development of functional terminal products; furthermore, high-value utilization of the tea tree purple bud resources is realized truly.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity tea tree purple bud anthocyanins, especially extracting tea tree purple buds through acidic ethanol, firstly removing impurities through organic solvent extraction degreasing and cation exchange resin pretreatment, and then through high-speed countercurrent A method for preparing high-purity purple bud tea tree anthocyanins by chromatographic separation and preparative high-performance liquid chromatography purification. Background technique [0002] Anthocyanins are a class of plant secondary metabolites with the basic core structure of 2-phenylbenzopyran. They have various biological activities such as anti-oxidation and free radical scavenging. They are one of the hot spots in the field of natural product development and utilization in recent years. Tea anthocyanins have various biological activities such as anti-oxidation, scavenging free radicals, detoxification and liver p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/065C07H1/08
CPCC07H1/08C07H17/065
Inventor 龚志华刘林峰肖文军
Owner HUNAN AGRICULTURAL UNIV
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