Method for low-pressure silica gel column chromatographic separation of capsaicin and dihydrocapsaicin

A technology of dihydrocapsaicin and silica gel column chromatography, which is applied in the separation/purification of carboxylic acid amide, ion exchange, ion exchange regeneration, etc., can solve the problems of high toxicity, high production cost, and serious environmental pollution, and achieve low toxicity, The effect of low cost and high product purity

Inactive Publication Date: 2011-04-20
HUNAN AGRICULTURAL UNIV +1
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Problems solved by technology

The method adopts the silica gel column chromatography method that silver nitrate is handled, and elutes with mixed solvents such as chloroform, ethyl acetate, because this method uses silver salt (silver nitrate) in a large amount, the production cost is high; Simultaneously this method uses chloroform etc. Solvent, high toxicity, serious environmental pollution

Method used

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  • Method for low-pressure silica gel column chromatographic separation of capsaicin and dihydrocapsaicin
  • Method for low-pressure silica gel column chromatographic separation of capsaicin and dihydrocapsaicin

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Embodiment 1

[0016] Embodiment 1: get capsicum total alkaloid 1g (total alkaloid content 97.8%), dissolve with 10ml acetone, 4g silica gel mix sample, go up in the column that 150g silica gel is housed, elute with sherwood oil / acetone=8: 2, every 30ml collects a part, paper chromatography qualitatively detects capsaicinoids, and the effluent containing capsaicins is analyzed by HPLC, the effluents of the same monomer capsaicin and dihydrocapsaicin are combined, and the solvent is recovered to obtain capsaicin 203mg, dihydrocapsaicin respectively. Hydrocapsaicin 91 mg, HPLC analysis content, respectively 98.1% and 98.5%, yields were 30.2% and 36.5%.

Embodiment 2

[0017] Embodiment 2: Get capsicum total alkaloid 1g (total alkaloid content 97.8%), dissolve with 10ml acetone, 5g silica gel mix sample, put on the column that 150g silica gel is housed, elute with sherwood oil / ethyl acetate=7:3 , collect one portion per 30ml, paper chromatography qualitatively detects capsaicin-like substances, and the effluent containing capsaicin-like substances is analyzed by HPLC, the effluents of the same monomer capsaicin and dihydrocapsaicin are combined, and the solvent is recovered to obtain 194mg capsaicin respectively , 87 mg of dihydrocapsaicin, the contents of HPLC analysis were 97.8% and 98.2% respectively, and the yields were 28.7% and 34.7% respectively.

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Abstract

The invention relates to a method for the low-pressure silica gel column chromatographic separation of capsaicin and dihydrocapsaicin. Capsaicin and dihydrocapsaicin can be obtained by the following main procedures: using capsaicinoids as a raw material, carrying out low-pressure silica gel column chromatographic separation, eluting with petroleum ether and other solvents, carrying out HPLC (high performance liquid chromatography) analysis and the like. Compared with the traditional method, the invention has the advantages of less environmental pollution, high product purity, low cost and the like, thereby being applicable to industrial production.

Description

technical field [0001] The invention relates to a method for separating capsaicin and dihydrocapsaicin by low-pressure silica gel column chromatography. Background technique [0002] Total capsaicin is composed of more than ten analogues such as capsaicin (60-70%) and dihydrocapsaicin (20-30%), but capsaicin is generally used in medical research. Because the structures and physical and chemical properties of capsaicin analogs are very close, it is difficult to separate the monomeric compounds. Chinese patent ZL200610068854.9 (a method for the purification and preparation of capsaicin monomer) introduces a method for producing capsaicin monomer from capsaicin total alkaloids. The method adopts the silica gel column chromatography method that silver nitrate is handled, and elutes with mixed solvents such as chloroform, ethyl acetate, because this method uses silver salt (silver nitrate) in a large amount, the production cost is high; Simultaneously this method uses chloroform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/20C07C233/18B01D15/08
Inventor 董新荣杨华
Owner HUNAN AGRICULTURAL UNIV
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