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Preparation method of arctiin

A technology of arctiin and burdock, which is applied in the field of arctiin preparation to achieve the effects of less pollution, favorable large-scale production operations, and low energy consumption

Inactive Publication Date: 2011-06-22
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity arctiin

Method used

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  • Preparation method of arctiin

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Experimental program
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Effect test

Embodiment 1

[0026] Get burdock dry ripe fruit 10Kg, add to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 2%, the extraction pressure is 20MPa, the temperature is 30°C, and CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 120min, the extract is obtained, the solvent is recovered under reduced pressure, and the ethyl acetate-water mixed solvent with a ratio of 10:2 is used for three-stage countercurrent extraction, the extracts are combined, the solvent is recovered under reduced pressure and Concentrate, add to HPD-700 macroporous adsorption resin column for adsorption, elute with 40% ethanol, collect 3 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add acetone to crystallize, separate crystallization, wash and dry. Obtain arctiin 50.3g, detect by HPLC, the purity is 95.7%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physi...

Embodiment 2

[0028] Get burdock dry ripe fruit 10Kg, add to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 5%, the extraction pressure is 40MPa, the temperature is 50°C, and CO 2 The flow rate is 3ml / g crude drug·min, the extraction time is 180min, the extract is obtained, the solvent is recovered under reduced pressure, and the mixed solvent of ethyl acetate-water with a ratio of 10:2 is used for 8-stage countercurrent extraction, the extracts are combined, the solvent is recovered under reduced pressure and Concentrate, add to H-50 macroporous adsorption resin column for adsorption, elute with 60% ethanol, collect 8 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add acetone to crystallize, separate crystallization, wash and dry. Obtain arctiin 57.2g, detect by HPLC, the purity is 94.4%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical ...

Embodiment 3

[0030] Get burdock dry ripe fruit 10Kg, add to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 3%, the extraction pressure is 30MPa, the temperature is 40°C, and CO 2 The flow rate is 2ml / g crude drug·min, the extraction time is 150min, the extract is obtained, the solvent is recovered under reduced pressure, and the mixed solvent of ethyl acetate-water with a ratio of 10:2 is used for 6-stage countercurrent extraction, the extracts are combined, the solvent is recovered under reduced pressure and Concentrate, add to CD-180 macroporous adsorption resin column for adsorption, elute with 50% ethanol, collect 5 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add acetone to crystallize, separate crystallization, wash and dry. Obtain arctiin 53.6g, detect through HPLC, and purity is 98.2%, UV, IR, MS, 2 HNMR, 13 The data characterizing its ph...

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Abstract

The invention relates to a preparation method of arctiin, which is simple to operate and has the advantages of low pollution and low energy consumption. The method comprises the following steps: taking dry ripe fruits of burdock,, adding into a CO2 supercritical extractor, extracting by using ethanol as an entrainer to obtain an extract, recovering the solvent while depressurizing, carrying out multistage countercurrent extraction by using an ethyl acetate-water (10:2) mixed solvent, merging the extract liquids, recovering the solvent while depressurizing, concentrating the solvent, adding the solvent to macroporous adsorbent resin columns to be adsorbed, eluting with ethanol, collecting the eluent, recovering ethanol while depressurizing, concentrating, adding acetone to crystallize, separating the crystals, washing and drying to obtain the arctiin. The method for preparing arctiin has the advantage of high product purity, and can easily implement industrial scale-up production.

Description

technical field [0001] The invention relates to a preparation method of arctiin, in particular to a preparation method of extracting arctiin from plants. Background technique [0002] Arctiin (Arctin), molecular formula: C 27 h 34 o 11 , molecular weight: 534.559, CAS accession number: 20362-31-6. It mainly exists in the Compositae plant Arctium lappa L., and the source of raw materials is abundant. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that arctiin has various activities such as anti-platelet aggregation, anti-inflammation, and inhibition of urinary protein excretion, and it is also used as a raw material for the synthesis of other active derivatives. [0005] The dried and mature fruit of Arctium lappa L., a plant in the Compositae family, is used as a traditional Chinese medicine, Arctium lappa L., which has the effects of evacuating wind-heat, clearing the lungs and rash, detoxifying and relieving the throat. [0006] I...

Claims

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Application Information

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IPC IPC(8): C07H15/26C07H1/08
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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