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Preparation method of hydroxyl-alpha-sanshool single substance

A technology of hydroxy-sanshool and sanshool, which is applied in the field of preparation of hydroxy-α-sanshool monomer, which can solve the problem of easy changes in light or room temperature, instability of hydroxy-α-sanshool, and restrictions on the research and application of Zanthoxylum bungeanum, etc. problems, to achieve the effect of low price, low production cost and mild conditions

Active Publication Date: 2021-02-05
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN106977416A discloses a method for preparing hydroxy-α-sanshool through ultraviolet irradiation and n-hexane extraction, but the method needs to carry out ultraviolet irradiation, and hydroxy-α-sanshool is very unstable, and it is very easy to change under light or room temperature
However, the preparation of high-purity, high-yield hydroxy-α-sanshool monomer is still blank, resulting in a single standard product for the detection of Zanthoxylum bungeanum, which limits the research and application of Zanthoxylum bungeanum to a large extent.

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1, the preparation method of hydroxyl-alpha-sanshool monomer of the present invention

[0058] The preparation method comprises the following steps:

[0059] (1) Preparation of Zanthoxylum bungeanum extract total extract

[0060] Take 2 kg of dried Zanthoxylum bungeanum powder, extract with a volume fraction of 95% ethanol aqueous solution for 48 hours, the ratio of solid to liquid is 1:10 (kg / L), extract 3 times, combine the extracts, discard the drug residue, and store the extracts at 50°C Concentrate under reduced pressure to obtain a concentrated solution, the volume of the concentrated solution is 1 / 5 of the extract, and the total extract of Zanthoxylum bungeanum extract is obtained.

[0061] (2) Enrichment of hydroxy sanshool mixture

[0062] Dilute the total extract of Zanthoxylum bungeanum extract obtained in step (1) with water until the volume fraction of ethanol is 20%, extract with ethyl acetate, the volume ratio of ethyl acetate and water is 1L...

Embodiment 2

[0067] Embodiment 2, the preparation method of hydroxyl-alpha-sanshool monomer of the present invention

[0068] The preparation method comprises the following steps:

[0069] (1) Preparation of Zanthoxylum bungeanum extract total extract

[0070] Take 2 kg of dried Zanthoxylum bungeanum powder, extract it with 85% ethanol aqueous solution for 48 hours, the ratio of solid to liquid is 1:8 (kg / L), extract 3 times, combine the extraction solution, discard the drug residue, and store the extraction solution at 50°C Concentrate under reduced pressure to obtain a concentrated solution, the volume of the concentrated solution is 1 / 5 of the extract, and the total extract of Zanthoxylum bungeanum extract is obtained.

[0071] (2) Enrichment of hydroxy sanshool mixture

[0072] Dilute the total extract of Zanthoxylum bungeanum extract obtained in step (1) with water until the volume fraction of ethanol is 20%, extract with ethyl acetate, the volume ratio of ethyl acetate and water is...

Embodiment 3

[0077] Embodiment 3, the preparation method of hydroxyl-alpha-sanshool monomer of the present invention

[0078] The preparation method comprises the following steps:

[0079] (1) Preparation of Zanthoxylum bungeanum extract total extract

[0080] Take 2 kg of dried Zanthoxylum bungeanum powder, extract it with 90% methanol aqueous solution for 48 hours, the ratio of solid to liquid is 1:10 (kg / L), extract 3 times, combine the extracts, discard the drug residue, and store the extracts at 50°C Concentrate under reduced pressure to obtain a concentrated solution, the volume of the concentrated solution is 1 / 5 of the extract, to obtain the total extract of Zanthoxylum bungeanum extract.

[0081] (2) Enrichment of hydroxy sanshool mixture

[0082] Dilute the total extract of Zanthoxylum bungeanum extract obtained in step (1) with water to a volume fraction of methanol of 20%, extract with ethyl acetate, the volume ratio of ethyl acetate to water is 1L:1L, repeat this extraction ...

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Abstract

The invention provides a preparation method of a hydroxyl-alpha-sanshool single substance, and belongs to the technical field of natural medicine extraction and separation. The preparation method comprises the following steps: (1) conducting leaching with low alcohol to obtain a pepper extract total extract; (2) conducting extracting by adopting ethyl acetate, and enriching a hydroxysanshool mixture by column chromatography; (3) removing impurities by adopting a freezing crystallization method, and enriching hydroxyl-alpha-sanshool; and (4) separating and purifying the hydroxyl-alpha-sanshool.The preparation method of the hydroxyl-alpha-sanshool single substance is simple and convenient to operate and has low technical requirements on operators; the conditions in the preparation process are mild, so that the stability of the hydroxyl-alpha-sanshool is guaranteed, and the hydroxyl-alpha-sanshool is very safe; and meanwhile, the hydroxyl-alpha-sanshool single substance prepared by the preparation method is high in purity, the purity of the prepared hydroxyl-alpha-sanshool single substance can reach 99% or above, and the hydroxyl alpha-sanshool single substance can be used as a standard substance of the hydroxyl alpha-sanshool single substance. The preparation method is low in cost, suitable for large-scale industrial popularization and good in application prospect.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of natural medicines, and in particular relates to a preparation method of hydroxy-α-sanshool monomer. Background technique [0002] Zanthoxylum L., a plant of the genus Zanthoxylum in the family Rutaceae, has a very long history as a traditional condiment and Chinese herbal medicine in my country. It is one of the "eight condiments" in China. The pungent taste is the most important flavor characteristic of Zanthoxylum bungeanum, and it is also the most important indicator to evaluate its quality. In addition, Zanthoxylum bungeanum is also a commonly used traditional Chinese medicine in my country. It has the functions of warming, relieving pain, antibacterial and insecticidal, and can be used to treat vomiting, diarrhea, ascariasis and other diseases. [0003] In the application of Zanthoxylum bungeanum, the most important thing is still its flavor. The unsaturated fatty amide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/20
CPCC07C231/24C07C233/20
Inventor 周先礼陈琳张政史波林赵镭黄帅
Owner SOUTHWEST JIAOTONG UNIV
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