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Hydroxy-beta-sanshool monomer preparation method

A technology of hydroxy sanshool and sanshool, which is applied in the field of natural medicine extraction, can solve the problems of restricting the research and application of numbing substances in peppercorns, and achieve the effects of low price, low production cost and high yield

Active Publication Date: 2016-04-13
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the extraction and preparation methods of the numbing substances of Zanthoxylum bungeanum mainly use supercritical CO 2 The numbing substance sanshool of pepper is extracted and separated. Most of the extracts are pepper oleoresin or essential oil. Only mixed hydroxyl sanshool can be obtained, but the hydroxyl-β-sanshool monomer of pepper cannot be efficiently separated and purified, to a large extent Restricted the research and application of Zanthoxylum bungeanum flavor substances

Method used

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Examples

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Effect test

Embodiment 1

[0045] A preparation method of hydroxy-beta-sanshool monomer, comprising the steps of:

[0046] ⑴Extraction of hydroxy sanshool mixture

[0047] Take 2 kg of dried Zanthoxylum bungeanum peel and crush it, extract it with an aqueous solution with a volume fraction of 95% ethanol for 48 hours, and extract 3 times at a liquid-to-solid ratio of 1:10, combine the extracts, discard the drug residues, and reduce the extracts at a temperature of 50°C. Concentrate under pressure to obtain a concentrated solution, the volume of the concentrated solution is 1 / 5 of the leaching solution, and the mixture of hydroxyl sanshools, that is, the crude product of piananthamide is obtained.

[0048] ⑵Enrichment of hydroxy sanshool mixture

[0049] Dilute the Zanthoxylum amide crude product obtained in step (2) with water until the volume fraction of ethanol is 20%, and separate and purify it by D101 macroporous adsorption resin column chromatography. When loading the sample, the adsorption rate is...

Embodiment 2

[0055] A preparation method of hydroxy-beta-sanshool monomer, comprising the steps of:

[0056] ⑴Extraction of hydroxy sanshool mixture

[0057] Take 2 kg of dried Zanthoxylum bungeanum pericarp and crush it, extract it with water with a volume fraction of 85% ethanol for 48 hours, the ratio of liquid to material is 1:8, extract 3 times, combine the extraction solution, discard the drug residue, and reduce the extraction solution at a temperature of 50°C. Concentrate under pressure to obtain a concentrated solution, the volume of the concentrated solution is 1 / 5 of the leaching solution, and the mixture of hydroxyl sanshools, that is, the crude product of piananthamide is obtained.

[0058] ⑵Enrichment of hydroxy sanshool mixture

[0059] Dilute the Zanthoxylum amide crude product obtained in step (2) with water until the volume fraction of ethanol is 20%, and separate and purify it by HP-20 macroporous adsorption resin column chromatography. , dynamic adsorption loading, th...

Embodiment 3

[0065] A method for preparing hydroxy-beta-sanshool monomer, comprising the steps of:

[0066] ⑴Extraction of hydroxy sanshool mixture

[0067] Take 2 kg of dried Zanthoxylum bungeanum peel and crush it, extract it with water with a volume fraction of 90% methanol for 48 hours, and extract 3 times with a liquid-to-solid ratio of 1:10, combine the extracts, discard the drug residue, and reduce the extract at a temperature of 50 °C. Concentrate under pressure to obtain a concentrated solution, the volume of the concentrated solution is 1 / 5 of the leaching solution, and the mixture of hydroxyl sanshools, that is, the crude product of piananthamide is obtained.

[0068] ⑵Enrichment of hydroxy sanshool mixture

[0069] Dilute the Zanthoxylum amide crude product obtained in step (2) with water to a volume fraction of methanol of 15%, and separate and purify it by AB--8 macroporous adsorption resin column chromatography. , dynamic adsorption loading, the adsorption rate is controll...

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Abstract

The invention provides a hydroxy-beta-sanshool monomer preparation method and belongs to the technical field of natural drug extraction. The preparation method effectively realizes extraction of a high-concentration hydroxy-beta-sanshool monomer from a Chinese prickly ash raw material. The preparation method comprises 1, extracting a hydroxysanshool mixture, 2, carrying out enrichment and pressure reduction condensation on the hydroxysanshool mixture to obtain hydroxysanshool mixture extract, 3, transforming hydroxy-beta-sanshool to improve hydroxy-beta-sanshool content of the hydroxysanshool mixture extract solution, 4, purifying the hydroxy-beta-sanshool to obtain a hydroxy-beta-sanshool monomer with purity of 70% or more, and 5, carrying out recrystallization to obtain a hydroxy-beta-sanshool monomer with purity of 98% or more. The preparation method is mainly used for preparing the hydroxy-beta-sanshool monomer.

Description

technical field [0001] The invention belongs to the technical field of natural medicine extraction. Background technique [0002] Zanthoxylum L. is a plant of the Rutaceae (Rutaceae) Zanthoxylum Linn. Zanthoxylum bungeanum fruit is one of the traditional "eight major condiments" in my country, and its spicy and numbing taste is the main flavor characteristic and the most important quality index. In addition, Zanthoxylum bungeanum is also a commonly used traditional Chinese medicine in my country, which can be used to treat vomiting, diarrhea, ascariasis, etc. External application can treat eczema, itching, promoting blood circulation and dissipating blood stasis. Has obvious pharmacological activity. [0003] Most of the pepper amides are chain unsaturated fatty acid amide structures, among which sanshool is the main component of pepper numbing, which can stimulate TRPV1, TRPA1 and so on. The amide substances in Zanthoxylum bungeanum are mainly hydroxy-α-sanshool and hydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C231/24C07C233/20
CPCC07C231/12C07C231/24C07C233/20
Inventor 周先礼黄帅张敬文单连海赵镭史波林
Owner SOUTHWEST JIAOTONG UNIV
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