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Method for extracting and purifying tangerine polymethoxyflavone

A technique of polymethoxylated flavonoids and a purification method, which is applied in the field of extraction and purification of active ingredients of agricultural by-products, can solve the problems of difficult industrialization, expensive purification equipment, complicated processes, etc., and achieves easy industrial production and simple and easy purification process , the effect of low investment

Active Publication Date: 2012-02-08
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to propose a reasonable purification process with high product purity and high yield in view of the defects of expensive purification equipment, complex process, high cost and difficulty in industrialization of the existing crude extract of citrus polymethoxyflavones , low cost, can meet the needs of food, health products, etc., and can be used for the extraction and purification of citrus polymethoxylated flavonoids in industrial production

Method used

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  • Method for extracting and purifying tangerine polymethoxyflavone
  • Method for extracting and purifying tangerine polymethoxyflavone
  • Method for extracting and purifying tangerine polymethoxyflavone

Examples

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Effect test

Embodiment 1

[0035] Embodiment 1: (extraction and purification method 1 of citrus polymethoxylated flavone crude extract)

[0036] (1) Extraction of citrus polymethoxylated flavonoids:

[0037] 1) Pretreatment of citrus peels: dry the citrus peels to a water content of ≤5%, grind them through a 30-mesh sieve, and set aside;

[0038] 2) Crude extraction and extraction of citrus polymethoxylated flavonoids: mix 500g of citrus peel powder and 5.0L of water, heat to 100°C for extraction for 1 hour, and filter to obtain a water extract; mix the water extract with n-hexane by volume Mixing and extracting at a ratio of 1:0.5; the extract was evaporated to dryness under reduced pressure at 40°C to obtain a crude extract of citrus polymethoxyflavones; through HPLC analysis, the crude extract contained 30.8% nobiletin, orange Cortex 22.7%;

[0039] (2) column chromatography purification of citrus polymethoxyflavone crude extract;

[0040] 1) Preparation of the crude extract solution: Dissolve 5 g...

Embodiment 2

[0044] Embodiment 2: (extraction and purification method 2 of citrus polymethoxylated flavone crude extract)

[0045] In this example, step (2) column chromatography purification of the crude extract of citrus polymethoxylated flavones;

[0046] 1) Preparation of the crude extract solution: Dissolving 5 g of the citrus polymethoxylated flavone crude extract in 500 ml of 30% ethanol solution;

[0047] 2) Packing of macroporous resin column: put the pretreated macroporous resin DM312 into the chromatography column to a column height of 20cm;

[0048]3) Adsorption of macroporous resin: 500ml of the crude extract solution was passed through the chromatographic column with a peristaltic pump at a flow rate of 1.5ml / min for 5.56h, and the effluent was collected; The total adsorption rate of the analysis column to polymethoxylated flavones is 80%;

[0049] 4) Elution, collection, concentration and drying of macroporous resin: use 500ml of 100% ethanol as the eluent; combine eluents...

Embodiment 3

[0051] Embodiment 3: (extraction and purification method 3 of citrus polymethoxylated flavone crude extract)

[0052] In this example, step (2) column chromatography purification of the crude extract of citrus polymethoxylated flavones;

[0053] 1) Preparation of the crude extract solution: Dissolve 5 g of the citrus polymethoxylated flavone crude extract in 500 ml of 40% ethanol solution;

[0054] 2) Macroporous resin packing: put the pretreated macroporous resin AB-8 into the chromatography column to a height of 15cm;

[0055] 3) Adsorption of macroporous resin: 500ml of the crude extract solution was passed through the chromatographic column with a peristaltic pump at a flow rate of 2.0ml / min for 4.17h, and the effluent was collected; The total adsorption rate of the analysis column to polymethoxylated flavones is 68%;

[0056] 4) Elution, collection, concentration and drying of macroporous resin: use 500ml of 60% ethanol as the eluent; combine the eluents from tubes 1 to...

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Abstract

The invention discloses a method for extracting and purifying tangerine polymethoxyflavone, which belongs to the technical field of extracting and purifying the effective components of farm and sideline products. The method comprises the following processing steps: (1) extracting the tangerine polymethoxyflavone, (2) carrying out column chromatography purification on the crude extract of the tangerine polymethoxyflavone and the like. Nobiletin and tangeretin in the crude extract of the tangerine polymethoxyflavone can respectively reach 30.8 percent and 22.7 percent in content; the purification effect of selected macroporous resin on the crude extract is higher; the total content of the macroporous resin can reach 74.1-82.1 percent; and the total recovery rate can reach 45.9-68.6 percent. Moreover, the method for extracting and purifying the tangerine polymethoxyflavone has the characteristics that equipment is simple, the process is reasonable and is easy to implement, the cost is low, and a product can meet the requirements of food, health care products and the like. The method can be popularized and applied to tangerine producing areas and biochemical enterprises.

Description

technical field [0001] The invention relates to the technical field of extraction and purification of active ingredients of agricultural by-products, in particular to a method for extracting and purifying active ingredients polymethoxylated flavonoids from citrus peels. Background technique [0002] We know that citrus is rich in flavonoids, among which polymethoxylated flavones are unique to citrus, Nobiletin (Nobiletin) and Tangeretin (Tangeretin) are the representatives, they are mainly distributed in citrus In the oil cells of the skin, the content is 0.4-0.6mg / g. Due to its planar structure, multiple methoxy groups, and low polarity, this kind of substance has various pharmacological effects such as anti-cancer, anti-inflammatory, anti-oxidation, anti-mutagenesis, and cholesterol-lowering effects, especially in anti-cancer The effect of aspect is stronger than other flavonoids. [0003] At present, the citrus polymethoxylated flavonoids are mainly extracted by solvent...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
Inventor 郑美瑜陆胜民夏其乐杨颖陈剑兵邢建荣
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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