Method for refining dihydroquercetin from larch

A technology of dihydroquercetin and larch, applied in the direction of organic chemistry and the like, can solve the problems of inconvenient continuous production of adsorbents, increase the number of crystallizations, large solvent consumption, etc., achieve high yield, simplify production steps, Low self-residue effect

Active Publication Date: 2013-10-23
PEKING UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has the following defects: the consumption of solvent is large, and toxic solvents such as ether and ketone need to be introduced; the purity of the crude product is low, and it is often necessary to further decolorize or increase the number of crystallization times to reduce the yield
Among them, ether, ketone or chlorine-containing solvents are often introduced in the extraction operation, which is highly toxic and costly; the adsorbent used in some adsorption methods is not convenient for continuous production, or it is easy to introduce impurities of the adsorbent itself into the final product

Method used

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  • Method for refining dihydroquercetin from larch
  • Method for refining dihydroquercetin from larch
  • Method for refining dihydroquercetin from larch

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Embodiment 1

[0038] Embodiment 1: refined dihydroquercetin

[0039] (1) Extraction: 100g of larch wood powder, add 1.5L of 95% ethanol aqueous solution by volume fraction, soak for 4h, heat to reflux for 2h (80°C), filter the extract; then add 1.0L of 95% ethanol aqueous solution by volume fraction , heated to reflux for 2h (80°C), the extract was filtered and combined with the previous one, concentrated under reduced pressure at 50°C until there was no alcohol smell, and 10g of extract was obtained.

[0040] (2) Purification: The extract obtained in step (1) is subjected to liquid phase adsorption separation with a small-porous resin MCI (SBC MCI GEL, 75-150 μM, type F). Sequentially eluted with ethanol aqueous solution with a volume fraction of 10%, 20%, 25%, and 30%, and each gradient eluted with 3 column volumes. The effluent was collected and concentrated in sections, and detected by TLC. The higher fractions (20-25% elution fraction) were combined to obtain 1.57 g of dihydroquerceti...

Embodiment 2

[0043] Embodiment 2: refined dihydroquercetin

[0044] (1) Extraction: 1000g of larch wood powder, add 5L of ethanol solution with a volume fraction of 95%, soak for 4h, heat to reflux for 2h (80°C), filter the extract; then add 5L of 95% ethanol solution, heat Reflux for 2h (80°C), filter the extract and combine it with the previous one, and concentrate under reduced pressure at 35°C until there is no alcohol smell, and 100g of extract is obtained.

[0045] (2) Purification: The extract obtained in step (1) is subjected to liquid phase adsorption separation with a small-porous resin MCI (SBC MCI GEL, 75-150 μM, type F). Sequentially eluted with ethanol aqueous solution with a volume fraction of 10%, 20%, 25%, and 30%, and each gradient eluted with 5 column volumes. The effluent was collected and concentrated in sections, and detected by TLC. The higher fractions of dihydroquercetin (20-25% elution fraction) were combined to obtain 15.6 g of dihydroquercetin crude product. T...

Embodiment 3

[0048] Embodiment 3: refined dihydroquercetin

[0049] (1) Extraction: 10000g of larch wood powder, add 80L of ethanol solution with a volume fraction of 95%, soak for 4h, heat and reflux for 2h (90°C), and filter the extract; add 60L of 95% ethanol solution with volume fraction, heat Reflux for 2h (90°C), filter the extract and combine it with the previous one, and concentrate under reduced pressure at 40°C until there is no alcohol smell, and 1000g of extract is obtained.

[0050] (2) Purification: The extract obtained in step (1) is subjected to liquid phase adsorption separation with a small-porous resin MCI (SBC MCI GEL, 75-150 μM, type F). Sequentially eluted with ethanol aqueous solution with a volume fraction of 10%, 20%, 25%, and 30%, and each gradient eluted with 5 column volumes. The effluent was collected and concentrated in sections, and detected by TLC. The higher fractions (20-25% elution fraction) were combined to obtain 160 g of dihydroquercetin crude product...

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Abstract

The invention discloses a method for refining dihydroquercetin from larch by using micro-porous resin. The method comprises the following steps: (1) after crushing the raw material larch wood, adding ethanol water solution to extract, collecting extracting solution and concentrating to obtain extract; (2) performing liquid phase adsorption separation on the extract by using micro-porous resin MCI, performing gradient elution by taking the ethanol water solution with volume fraction of 0-30 percent as an eluant, collecting and combining elution components with volume fraction of 20-25 percent, concentrating and drying to obtain a dihydroquercetin rough product; and (3) recrystallizing the dihydroquercetin rough product to obtain refined dihydroquercetin. According to the method, environment-friendly solvents such as water and ethanol are adopted, are pollution-free and can be recycled; the used adsorbent micro-porous resin introduces less impurities and can be reused for times; the obtained product has purity of greater than 99 percent and has no toxic ingredient residues, and the pharmaceutical-grade raw material can be directly obtained. The method has the advantages of simple route, economy, environmental friendliness and high yield and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for refining dihydroquercetin from larch. Background technique [0002] Dihydroquercetin (taxifolin, dihydroquercetin), also known as taxifolin, taxifolin, taxifolin, molecular formula C 15 h 12 o 7 , molecular weight: 304.25, structural formula: see formula I. It is a dihydroflavonol compound with the chemical name 5,7,3',4'-tetrahydroxydihydroflavonol. Dihydroquercetin widely exists in pinaceae plants, such as maritime pine, larch, and Douglas fir, and is the flavonoid compound with the largest content in larch, with a content of about 0.3-5.7%. [0003] [0004] (Formula I) [0005] Dihydroquercetin has a strong antioxidant capacity, can effectively eliminate excess free radicals from the human body, and promote the permeability of capillaries. Its antioxidant properties are superior to many existing antioxidants, and there is no toxicity report, so it is widely used as an antioxidant additive in foods such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/32C07D311/40
Inventor 叶敏苗文娟刘春芳乔雪程晓伟
Owner PEKING UNIV
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