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A method for separating and preparing 5-hydroxymethylfurfural from Shengmai Fang

A technology of hydroxymethylfurfural and pulse prescription, which is applied in the field of natural medicinal chemistry, can solve the problems of separation and preparation efficiency and product purity, and increase the difficulty of 5-hydroxymethylfurfural, so as to achieve easy control of operating process conditions and ensure safety The effect of sex and process method is simple

Active Publication Date: 2016-09-14
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, the complex chemical components in the traditional Chinese medicine compound and the complex physical and chemical changes of each component in the compatibility process make it more difficult to separate and prepare 5-hydroxymethylfurfural from the traditional Chinese medicine compound, and the separation and preparation efficiency and product Purity is greatly affected

Method used

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  • A method for separating and preparing 5-hydroxymethylfurfural from Shengmai Fang
  • A method for separating and preparing 5-hydroxymethylfurfural from Shengmai Fang
  • A method for separating and preparing 5-hydroxymethylfurfural from Shengmai Fang

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Embodiment 1

[0036] (1) The composition of Shengmai Fang in this embodiment is: Codonopsis 300g, Ophiopogon japonicus 200g, Schisandra chinensis 100g, the above three flavors are crushed into coarse powder, decocted twice with water, each decocting 2h, the amount of water used for the two times is 3200mL respectively , 2400mL. The extracts were combined and filtered, and the filtrate was concentrated to obtain a viscous extract containing 5-hydroxymethylfurfural.

[0037] (2) Get the pretreated D-101 type macroporous resin and pack it into a glass column. The column volume is 23mL, and the crude extract obtained in step (1) is loaded into the sample, and the loading amount is 20g. After adsorption, first Remove impurities with 125 mL of water (about 5 times the column volume), then elute with 200 mL of 30% ethanol-water solution (about 8 times the column volume) at a flow rate of 1 mL / min, collect the eluate in separate tubes, identify by liquid chromatography, and combine The eluate cont...

Embodiment 2

[0041] (1) Get the pretreated AB-8 type macroporous resin and pack it into a glass column. The column volume is 20mL. The crude extract obtained from step (1) in Example 1 is loaded into the sample, and the sample size is 12g. Finally, remove impurities with 100 mL of water (about 5 times the column volume), then elute with 160 mL of 30% ethanol-water solution (about 8 times the column volume) at a flow rate of 1 mL / min, collect the eluate in separate tubes, and perform liquid chromatography Identify, combine the eluate containing 5-hydroxymethylfurfural, and concentrate the eluate to obtain 0.193 g of macroporous resin enrichment. Wherein, the detection condition of liquid chromatography is the same as embodiment 1.

[0042] (2) Using medium-pressure preparative chromatography to separate and purify the macroporous resin enrichment obtained in step (1). Use reversed-phase silica gel C18 column (23*4.9cm i.d.), take 496.9mg of the macroporous resin enrichment obtained in step...

Embodiment 3

[0044] (1) The composition of Shengmai Fang in this example is: 300g ginseng, 300g Ophiopogon japonicus, 200g schisandra, the above three flavors are crushed into coarse powder, decocted twice with water, each decocting 2h, the amount of water used for the two times is 4000mL respectively , 3000mL. The extracts were combined and filtered, and the filtrate was concentrated to obtain a viscous extract containing 5-hydroxymethylfurfural.

[0045] (2) Get the pretreated D-101 type macroporous resin and pack it into a glass column, the column volume is 25mL, and the crude extract obtained in step (1) is loaded into the sample, and the loading amount is 20g. After adsorption, first Remove impurities with 125 mL of water (about 5 times the column volume), then elute with 200 mL of 30% ethanol-water solution (about 8 times the column volume) at a flow rate of 1 mL / min, collect the eluate in separate tubes, identify by liquid chromatography, and combine The eluate containing 5-hydroxy...

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Abstract

The invention discloses a method for separation and preparation of 5-hydroxymethylfurfural from a Shengmai prescription. The method comprises the following steps: (1) with the Shengmai prescription as a raw material, extracting with water, an ethanol-water solution or a methanol-water solution, and concentrating the extract liquid to obtain a crude extract containing 5-hydroxymethylfurfural; (2) adsorbing the crude extract obtained in the step (1) with a macroporous resin, eluting with water, and then eluting with a 20%-40% ethanol-water solution; and merging the eluates identified to contain 5-hydroxymethylfurfural through liquid chromatography, and concentrating the eluate to obtain a macroporous resin enriched matter; and (3) separating the macroporous resin enriched matter obtained in the step (2) with middle and low pressure preparative chromatography or high-speed countercurrent chromatography, collecting a fraction containing 5-hydroxymethylfurfural, concentrating, drying, and thus obtaining 5-hydroxymethylfurfural. The method achieves separation and preparation of 5-hydroxymethylfurfural from the traditional Chinese medicine compound prescription, is simple in method and high in efficiency, and can obtain the monomer finished product with the purity of greater than 90% at one time.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a method for separating and preparing 5-hydroxymethylfurfural from Shengmai Fang. Background technique [0002] 5-hydroxymethylfurfural (5-hydroxymethylfurfural, referred to as 5-HMF), also known as 5-hydroxymethyl-2-furfural, 5-hydroxymethyl-2-furfural, etc., the molecular formula is C 6 h 6 o 3 , a colorless needle-like crystal with a chamomile scent, is a small molecular compound containing a furan ring. It is one of the common ingredients in Chinese herbal medicines and traditional Chinese medicine compound prescriptions, and is also widely found in raisins, dairy products, honey, cakes and other foods. Its structural formula is: [0003] [0004] 5-Hydroxymethylfurfural is generally considered to be a degradation product of starch and polysaccharides. It has been reported in the literature that it is harmful to human striated muscles and viscera, has neurot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 楚楚
Owner ZHEJIANG UNIV OF TECH
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