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Method for preparing arctiin

A technology for arctiin and arctifolia seed is applied in the field of preparation of arctiside, and can solve the problems of low arctiside content, serious pollution, disadvantageous to large-scale production operations and the like

Inactive Publication Date: 2010-06-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, the extraction and separation method of arctiin mainly adopts organic solvent method, etc., but the content of arctiin obtained by these extraction processes is low, the pollution in the production process is serious, and it is unfavorable for large-scale production operations

Method used

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  • Method for preparing arctiin

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Experimental program
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Effect test

Embodiment 1

[0018] Get burdock seed coarse powder 10Kg, add sherwood oil 3 times volume of its weight and heat reflux for 1 hour, discard sherwood oil, dregs evaporate to dryness, add 60% ethanol 3 times volume of its weight and reflux 1 time, each time 1 hours, combine the medicinal solution, filter, recover ethanol under reduced pressure and concentrate, add an equal volume of water, stir evenly, filter, take the filtrate, add to AB-8 macroporous adsorption column for adsorption, elute with 10% ethanol, collect 3 times the eluate of the column volume, recover the ethanol under reduced pressure and concentrate, add dichloromethane-ethyl acetate-methanol (4:4:1) to crystallize, separate the crystals, add methanol to recrystallize, separate, wash and dry. 311.3 g of arctiin was obtained, and the purity was 99.4% as detected by HPLC.

Embodiment 2

[0020] Get Burdock Fructus coarse powder 10Kg, add the sherwood oil of 8 times of its weight volume and heat and reflux for 3 hours, discard the sherwood oil, dregs evaporate to dryness, add 60-90% ethanol of 10 times of its weight and volume to reflux 3 times, After 3 hours, combine the medicinal solution, filter, recover ethanol under reduced pressure and concentrate, add an equal volume of water, stir evenly, filter, take the filtrate, add to H-103 macroporous adsorption column for adsorption, and elute with 50% ethanol , collect the eluate of 8 times the volume of the column, recover the ethanol under reduced pressure and concentrate, add dichloromethane-ethyl acetate-methanol (4:4:1) to crystallize, separate the crystals, add methanol to recrystallize, separate, wash, After drying, 265.3 g of arctiin was obtained, which was detected by HPLC with a purity of 98.2%.

Embodiment 3

[0022] Get Burdock Fructus coarse powder 10Kg, add the sherwood oil of its weight 5 times of volume and heat and reflux for 2 hours, discard the sherwood oil, dregs evaporate to dryness, add 80% ethanol of its weight of 8 times of volume and reflux 2 times, each 2 hours, combine the liquid medicines, filter, recover ethanol under reduced pressure and concentrate, add an equal volume of water, stir evenly, filter, take the filtrate, add to D101 macroporous adsorption column for adsorption, elute with 30% ethanol, collect 5 times Measure the eluate of the column volume, recover ethanol under reduced pressure and concentrate, add dichloromethane-ethyl acetate-methanol (4:4:1) to crystallize, separate the crystals, add methanol to recrystallize, separate, wash, and dry to obtain burdock 302.3g of glycosides, detected by HPLC, the purity is 98.0%.

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Abstract

The invention relates to a method for preparing arctiin, which has the advantages of simple and convenient operation, light pollution and low equipment input. The method comprises the following process steps: taking crude powder of great burdock achene, adding petroleum ether of which the volume is 3 to 8 times weight of the crude powder, and heating and refluxing for 1 to 3 hours; discarding the petroleum ether, volatilizing dreg of decoction to dryness, adding 60 to 90 percent ethanol of which the volume is 3 to 10 time weight of the dreg of decoction, refluxing for 1 to 3 times, and refluxing for 1 to 3 hours each time; merging liquor, filtering, recovering the ethanol under reduced pressure, concentrating the liquor, adding water with equal volume, uniformly stirring, and filtering; taking filtrate, adding the filtrate to a macroporous adsorption column for adsorption, eluting with 10 to 50 percent ethanol, and collecting elution of which the volume is 3 to 8 times volume of the column; and recovering the ethanol under reduced pressure, concentrating the elution, and adding dichloromethane, ethyl acetate and methanol (4:4:1) for crystallization. The arctiin prepared by the method has high purity and is easy for industrial amplification.

Description

technical field [0001] The invention relates to a method for preparing arctiin, in particular to a method for extracting arctiin from plants. Background technique [0002] Arctiin (Arctiin), alias: Arctiin. Molecular formula: C 27 h 34 o 11 , molecular weight: 534.559, CAS accession number: 20362-31-6, the structural formula is as follows: [0003] [0004] Arctiin is a natural compound, which has various physiological activities such as anticancer and vasodilation, and is widely found in various plants of Compositae. [0005] Burdock fruit is the fruit of Arctium lappa L., a plant of Compositae. It has the effects of dispelling wind-heat, expelling lung and clearing rash, detoxifying and relieving sore throat. Which contains a lot of arctiin. [0006] In the prior art, the extraction and separation methods of arctiin mainly use organic solvent methods, etc., but the content of arctiin obtained by these extraction processes is low, the pollution is serious in the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/26C07H1/08
Inventor 刘东锋范淦彬杨成东
Owner NANJING ZELANG MEDICAL TECH
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