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Separation and purification method of atisine chloride atractydin monomers

A technology for separation and purification of atractylodes, which is applied in the field of separation and purification of atractylodes monomers. It can solve the problems such as the separation process of high-purity atractylodes monomers, and achieve the effects of easy cost control, good solubility and simple operation.

Active Publication Date: 2017-05-17
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no relevant report on the separation process of high-purity atractylodes atractylodes monomer

Method used

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  • Separation and purification method of atisine chloride atractydin monomers
  • Separation and purification method of atisine chloride atractydin monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A method for separation and purification of atractylodes monomer, comprising the following process steps:

[0033] A. Raw material extraction

[0034] Crush 1 kg of Atractylodes atractylodis into particles with a diameter of about 3mm, add 5L of ethanol solution with a volume percentage of 95%, extract twice at 50°C for 2 hours each time, filter, collect, and combine the filtrates, concentrate to no alcohol, and the volume is about 300mL.

[0035] B. Extraction

[0036] The concentrated solution of step A was extracted three times with ethyl acetate at a volume ratio of 1:1, and the ethyl acetate was partially concentrated to a small volume.

[0037] C. Sample mixing and drying

[0038] Add about 50 grams of silica gel (60-80 mesh) to the ethyl acetate part to mix the sample, and dry it with air at 50°C to obtain 67 grams of dried mixed sample silica gel.

[0039] D. Silica gel column chromatography

[0040] Put the mixed sample into the packed silica gel (200-300 ...

Embodiment 2

[0047] A method for separation and purification of atractylodes monomer, comprising the following process steps:

[0048] A. Raw material extraction

[0049] Crush 5 kg of Atractylodes atractylodis into particles with a diameter of about 3mm, add 30L of ethanol solution with a volume percentage of 95%, extract twice at 50°C for 2 hours each time, filter, collect, and combine the filtrates, concentrate until alcohol-free, volume About 1.5L.

[0050] B. Extraction

[0051] The concentrated solution of step A was extracted three times with ethyl acetate at a volume ratio of 1:1, and the ethyl acetate was partially concentrated to a small volume.

[0052] C. Sample mixing and drying

[0053] Add about 280 grams of silica gel (60-80 mesh) to the ethyl acetate part to mix the sample, and dry it with air at 50°C to obtain 350 grams of dried mixed sample silica gel.

[0054] D. Silica gel column chromatography

[0055] Put the mixed sample into the packed silica gel (200-300 mesh...

Embodiment 3

[0061] A method for separation and purification of atractylodes monomer, comprising the following process steps:

[0062] A. Raw material extraction

[0063] Crush 25 kg of Atractylodes atractylodis into particles with a diameter of about 3 mm, add 125 L of ethanol solution with a volume percentage of 95%, extract 3 times at 50 ° C, each time for 2 hours, filter, collect, and combine the filtrates, concentrate to no alcohol, volume About 10L.

[0064] B. Extraction

[0065] The concentrated solution of step A was extracted three times with ethyl acetate at a volume ratio of 1:1, and the ethyl acetate was partially concentrated to a small volume.

[0066] C. Sample mixing and drying

[0067] Add about 1.3 kg of silica gel (60-80 mesh) to the ethyl acetate portion to mix the sample, and dry it with air at 50°C to obtain 1.7 kg of dried mixed sample silica gel.

[0068] D. Silica gel column chromatography

[0069] Put the mixed sample into the packed silica gel (200-300 mesh, ...

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Abstract

The invention discloses a separation and purification method of atisine chloride atractydin monomers. The method includes: using an ethanol solution to perform heating extraction on rhizoma atractylodis for 2-3 times, combining filtrate and concentrating until no alcohol exists; B, extracting the concentrated solution with ethyl acetate for 2-4 times, and concentrating the ethyl acetate; C, adding silica gel into the ethyl acetate, and performing sample mixing and drying; D, loading the mixed sample into a mounted silica gel column for silica gel column chromatography, eluting with pure petroleum ether, and using a thin-layer chromatography point plate to confirm and collect production sections; E, concentrating the collected eluted production sections, freezing to separate out crystals, and using a Buchner funnel to fast filter the atisine chloride atractydin crystals while the crystals are cold, wherein HPLC detection shows that the purity of the crystals can reach above 99%, and the crystals can be used as the comparison products of content measuring. The separation and purification method has the advantages that the method is simple in process, short in production cycle, easy in cost control and suitable for industrial production, organic reagents can be recycled, and the obtained atisine chloride atractydin monomers are high in purity.

Description

technical field [0001] The invention belongs to the field of separation and purification of traditional Chinese medicine monomers, and in particular relates to a method for separation and purification of atractylodes monomers. Background technique [0002] Atractylodes (scientific name: Atractylodes Lancea (Thunb.) DC.): Atractylodes Lancea is a perennial herb of the Asteraceae family. The rhizome of Atractylodes atractylodes is used as medicine. It is pungent and bitter, and has the property of warming and drying. Damp invigorating the spleen needs medicine. Therefore, it is most suitable for symptoms such as abdominal fullness, drowsiness and fatigue, poor appetite, nausea and diarrhea, white and greasy tongue coating caused by dampness and turbidity resistance and spleen failure. It is often used with Magnolia officinalis, which can not only enhance the effect of removing dampness, but also promote Qi to eliminate fullness and improve curative effect. [0003] Atractyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/36
CPCY02P20/582C07D307/36
Inventor 白兰辉陈冲张政严熏刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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