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Method for preparing arctiin

The technology of arctiside and arctium seed is applied in the field of preparation of natural medicines, and can solve the problems of low degree of separation automation, long separation process, difficult recovery and utilization of a solvent system, etc., and achieves convenient automatic production, reduced energy consumption, and convenient recovery. and recycling effects

Inactive Publication Date: 2012-07-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a simple extraction and separation, continuous operation and convenient solvent for the shortcomings of the existing arctiin separation and preparation process, such as long separation process, low degree of separation automation, and difficult recycling of the used solvent system. Method for preparing high-purity arctiin through recycling

Method used

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  • Method for preparing arctiin
  • Method for preparing arctiin

Examples

Experimental program
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Effect test

Embodiment 1

[0022] After crushing 50 g of Arctium Fructus into a 60-mesh coarse powder, add 10 times the amount of water to reflux for extraction twice for 2 hours, and combine the filtrates.

[0023] The obtained extract was directly entered into the HP-20 macroporous adsorption resin adsorption column for adsorption and enrichment, and then successively eluted with four gradients of water and mass concentrations of 30%, 60%, and 95% ethanol, and the eluent was washed with High performance liquid chromatography (HPLC) for analysis. HPLC detection column model: Zorbax SB-C18, 250mm×4.6mm I.D., 5μm and pre-column model: 10mm×4.6mm I.D., 5μm. The analysis conditions are: the mobile phase is (A) methanol, and (B) the mass fraction is 0.5% acetic acid. Gradient elution is within 0-25 minutes, the volume fraction of mobile phase (A) is from 30% to 90%; the volume fraction of mobile phase (B) is from 70% to 10%. Flow rate: 0.8 ml / min; UV absorption wavelength: 280nm; column temperature: 30°C....

Embodiment 2

[0027] After crushing 50 g of burdock fruit into a 60-mesh coarse powder, add 15 times the amount of water to reflux for extraction twice for 2 hours, and combine the filtrates.

[0028] The obtained extract is directly entered into the HP-20 macroporous adsorption resin adsorption column for adsorption and enrichment, and then sequentially eluted with water and four gradients with mass concentrations of 30%, 60%, and 95% methanol respectively. Analysis by HPLC. HPLC detection column model: Zorbax SB-C18, 250mm×4.6mm I.D., 5μm and pre-column model: 10mm×4.6mm I.D., 5μm. The analysis conditions are: the mobile phase is (A) methanol, and (B) the mass fraction is 0.5% acetic acid. Gradient elution is within 0-25 minutes, the volume fraction of mobile phase (A) is from 30% to 90%; the volume fraction of mobile phase (B) is from 70% to 10%. Flow rate: 0.8 ml / min; UV absorption wavelength: 280nm; column temperature: 30°C. The 60% methanol eluate containing arctiin was collected a...

Embodiment 3

[0032] After crushing 50 g of Arctium Fructus into a 60-mesh coarse powder, add 10 times the amount of water to reflux for extraction twice for 2 hours, and combine the filtrates.

[0033] Put the obtained extract directly into the HP-20 macroporous adsorption resin adsorption column for adsorption and enrichment, first elute with water and 30% ethanol, then use water-saturated ethyl acetate eluent, switch the six-way valve, and water-saturated The ethyl acetate eluent was switched to the sample loop in countercurrent chromatography.

[0034] The resulting 60% ethanol eluate containing arctiin was separated by countercurrent chromatography using a two-phase system of ethyl acetate-5% aqueous solution of sodium chloride as a solvent system, with ethyl acetate as the upper phase and 6% chlorine An aqueous solution of sodium chloride was the lower phase.

[0035]Turn on the countercurrent chromatography (900 rpm, column volume 270mL), inject the sample, switch to the macroporous...

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Abstract

The invention discloses a method for preparing arctiin, which comprises the following steps of: crushing burdock and extracting the crushed burdock by using water or alcoholic solution; allowing the extract to directly enter an absorption column to perform adsorption and enrichment, eluting the product with the water and the alcoholic solution in turn, and performing concentration under reduced pressure to obtain arctiin fraction; and performing countercurrent chromatographic separation on the arctiin fraction by using a two-phase system formed by aqueous solution consisting of a single organic solvent and salt to obtain salt arctiin fraction, and performing adsorption to remove the salt by using macroporous adsorption resin or ion exchange resin. The method has the advantages of simple process, continuous operation, contribution to automation and recovery and recycling of the solvent, and suitability for industrial mass production.

Description

technical field [0001] The invention relates to a preparation method of natural medicine, in particular to a preparation method of arctiin (also known as arctiin, English name Arctiin). Background technique [0002] Burdock (Arctium lappa L.) is a plant of the genus Arctium in the Compositae family. It is a traditional medicinal plant. Its fruit (burdock seed), leaves and roots are used as medicine. Burdock root is also used as a vegetable in Japan and Europe. Burdock Fructus is a commonly used traditional Chinese medicine for both medicine and food. It has the effects of pungent and cool solution, dispelling wind and heat dissipation, and clearing heat and detoxification. It is used for wind-heat cold, cough, phlegm, and measles. It is recorded in the Chinese Pharmacopoeia that it is used as a prescription ingredient to treat diseases such as wind-heat cold, sore throat, opaque rash, carbuncle and sore. Arctiin is a main active substance in Arctium Fructus, and its content...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/26C07H1/08
Inventor 吴世华郭梦喆
Owner ZHEJIANG UNIV
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