Method for separating burdock oil, arctiin, arctigenin, lappaol E and lappaol H from burdock

A technique for burdock seed oil and burdock aglycone is applied in the fields of burdock phenol E and burdock phenol H, and the separation of burdock seed oil, burdock glycosides, and burdock aglycone can solve the problems caused by the inability to select chemical components, the large amount of organic solvents and the influence of the environment. Large and other problems, to achieve the effect of good market prospects, high separation efficiency, and resource saving

Active Publication Date: 2016-06-15
CHONGQING KERUI PHARMA GRP
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  • Abstract
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Problems solved by technology

Patent CN1000443493C provides a method for preparing arctiin and arctigenin. This patent adopts organic solvent degreasing and polyamide column chromatography to obtain arctium oil, and also obtains a mixture of arctiin and its aglycon. However, this process uses organic solvents to extract the medicinal materials of Arctium Fructus, which consumes a large amount of organic solvents and has a great impact on the environment, and the obtained arctiin and arctigenin are a mixture, and corresponding chemical components cannot be selected to form a mixture according to the treatment characteristics.
[0004] Therefore, in order to further modernize traditional Chinese medicine and improve the application range and application effect of lignans, it is necessary to separate the lignans from Arctium Fructus to obtain their main active components. They are applied in different proportions according to the needs, but at present there is no method to make full use of the burdock fruit medicinal material to obtain burdock oil, arctiin, arctigenin and other lignan chemical components at the same time

Method used

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  • Method for separating burdock oil, arctiin, arctigenin, lappaol E and lappaol H from burdock
  • Method for separating burdock oil, arctiin, arctigenin, lappaol E and lappaol H from burdock

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Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1 burdock fruit defatting prepares burdock seed oil

[0021] Grind burdock fruit into a coarse powder that can pass through a 10-mesh sieve, and use CO 2 The supercritical extraction equipment degreases for 6 hours to obtain burdock seed oil and defatted burdock seed powder. CO 2 The technological conditions of supercritical extraction are: extraction pressure 30MPa, extraction temperature 40°C, separation pressure 10MPa, separation temperature 40°C, carbon dioxide flow rate 500L / h.

Embodiment 2

[0022] The chemical composition analysis of embodiment 2 burdock seed oil

[0023] (1) Extraction of volatile oil components in burdock seed oil

[0024] Utilize the steam distillation method to extract the volatile components in the burdock seed oil, accurately weigh 35.0g of the burdock seed oil, add 165mL of 5% sodium chloride solution in the round bottom flask with a material-to-liquid ratio of 1:5, heat, and remove from the condenser Start timing when the first drop of liquid is dripped from the nozzle at the lower end, control the temperature, keep a slight boiling state, and distill for 5 hours. After fully cooling, absorb the upper layer of oil, dry it in a water bath at 40°C, and weigh it for GC-MS analysis.

[0025] (2) Methylation of fatty acid components in burdock seed oil

[0026] Due to the high boiling point of fatty acid components, methyl ester derivatization is now carried out to reduce its boiling point and meet the detection requirements of GC-MS. Step ...

Embodiment 3

[0033] The preparation method of embodiment 3 arctiin, arctigenin, arctol E and arctol H

[0034] (1) The defatted burdock fruit powder obtained in Example 1 was subjected to reflux extraction for 3 to 4 times, and the extracted extract was filtered with a 150 to 300 mesh sieve, and the filtrate was combined and concentrated to obtain the extract; wherein, the extract Be the hydroalcoholic solution that mass concentration is 95%, the use quality of described hydroalcoholic solution is 10 times of described defatted burdock fruit powder during each extraction, and each extraction time is 2 hours;

[0035] (2) Add CH 2 Cl 2 (2.0L) was extracted 3 times, the extract was collected and concentrated under reduced pressure to obtain CH 2 Cl 2 Crude extract extract (450.0g).

[0036] (3) To CH 2 Cl 2 Add mixed sample silica gel to the crude extract extract, carry out silica gel column chromatography, utilize dichloromethane-methanol system to analyze the CH 2 Cl 2 The crude ex...

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PUM

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Abstract

The invention provides a method for separating burdock oil, arctiin, arctigenin, lappaol E and lappaol H from burdock. The method for separating the burdock oil, arctiin, arctigenin, lappaol E and lappaol H from the burdock comprises the following steps: firstly degreasing burdock through CO2 supercritical fluid extraction, separating to obtain the burdock oil and degreased burdock powder, carrying out water-alcohol extraction and concentration on the degreased burdock powder to obtain extract, carrying out CH2Cl2 extraction on the extract, loading the extract onto a silica gel column to be subjected to chromatography, carrying out dichloromethane-methanol gradient elution, carrying out thin-layer chromatography, and purifying, so as to obtain the arctiin, lappaol E, arctigenin and lappaol H. The method provided by the invention has the advantages that multiple products can be separated by adopting one continuous route only, raw materials are fully utilized, resources are saved, a degreasing process does not pollute the environment, the obtained burdock oil has high nutritive value, and the arctiin, arctigenin, lappaol E and lappaol H are high in purity and can be independently or mixed with other substances to be applied to the medicinal and edible field as raw materials.

Description

technical field [0001] The invention belongs to the technical field of separation and extraction, and relates to a method for separating burdock seed oil and lignan compounds from burdock seeds, in particular to a method for separating burdock seed oil, arctiin, arctigenin, and arctol E from burdock seeds. and arctol H methods. Background technique [0002] Arctium Fructus is the dry and mature fruit of the biennial herb Arctium (Arctiumlappa L.) in the Compositae family. It is widely distributed in East Asian countries. The efficacy of this medicine is included in the previous editions of the "Chinese Pharmacopoeia". Modern pharmacological studies have proved that burdock fruit has anti-inflammatory, anti-tumor, blood pressure-lowering and immune-regulating activities, and its chemical components mainly contain volatile oils and lignans, of which lignans mainly include arctiin, arctigenin, Phenol E, burdock phenol H. The chemical components of burdock oil, arctigenin, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/26C07H1/08C07D307/33C11B1/10
CPCC07B2200/07C07D307/33C07H1/08C07H15/26C11B1/104Y02P20/54
Inventor 刘睿斌刘俊敏周在富张起辉宋少辉苏其果蒋蒨林泉松吴华孙宗良张育珍郑阳
Owner CHONGQING KERUI PHARMA GRP
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