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Method for separating capsaicinoids monomers from capsaicinoids compounds

A technology of capsaicin and compounds, which is applied in the field of separation of capsaicin monomers and capsaicin monomers, can solve the problems of large consumption of solvents and fillers, unsuitability for large-scale production, unfavorable environmental friendliness, etc., and achieves simple operation and high efficiency. The effect of choosing separation ability and broad application prospects

Active Publication Date: 2012-08-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The above patents or patent applications provide the separation and purification method of capsaicin monomer from different angles, but due to the constraints of production factors, the separation and purification by chromatographic column elution or macroporous resin is more time-consuming, and subsequent steps (including recrystallization) etc.) The consumption of solvent and filler is large, and it is not suitable for large-scale production; methods such as adding silver ion complexing agent are loaded down with trivial details and complicated operations, and a large amount of utilization of organic solvents is also not conducive to environmental friendliness

Method used

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  • Method for separating capsaicinoids monomers from capsaicinoids compounds

Examples

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Effect test

Embodiment 1

[0046] Commercially available capsaicin compounds (wherein the total weight percent of capsaicin and dihydrocapsaicin are 92%) and sulfolane aqueous solution (sulfolane molar fraction is 20%) are made into a capsaicin compound concentration of 3 grams per liter of stock solution , with dodecane as extractant, with sulfolane aqueous solution (sulfolane mole fraction is 20%) as detergent, the flow ratio between raw material liquid, extractant, detergent three is 0.3: 20: 1, at 30 ℃ figure 1 Fractional extraction is carried out in the fractionation extraction device shown (there are 15 stages in the extraction section and 6 stages in the washing section), the raffinate is collected, water and organic solvents are removed by vacuum concentration, washed with water and dried to obtain the final product. Through HPLC analysis, the absolute purity of capsaicin in the final product is 98.9%, the relative content of capsaicin:dihydrocapsaicin is 99.1:0.9, and the yield is 98.7%.

Embodiment 2

[0048] Commercially available capsaicin compound (wherein the total weight percent of capsaicin and dihydrocapsaicin is 92%) and aqueous methanol (methanol molar fraction is 95%) is made into the stock solution that capsaicin compound concentration is 50 g / liter , with 1-octene as extractant, methanol aqueous solution (methanol mole fraction is 95%) as detergent, the flow ratio between raw material liquid, extractant and detergent is 6:50:1, at 55°C exist figure 1 Fractional extraction is carried out in the fractionation extraction device shown (17 stages of extraction section and 3 stages of washing section), the raffinate is collected, water and organic solvent are removed by vacuum concentration, washed with water and dried to obtain the final product. Through HPLC analysis, the absolute purity of capsaicin in the final product is 98.3%, the relative content of capsaicin:dihydrocapsaicin is 98.8:1.2, and the yield is 99.0%.

Embodiment 3

[0050] Extract the chili peel powder with ethanol several times, concentrate the filtrate, add alcohol with a volume fraction of 70% and stir under warm conditions, and obtain capsaicin and dihydrocapsaicin after concentration and distillation of dilute alcohol dissolved in capsaicin compounds The total weight percentage is the solid capsaicin compound of 78%, and the solid capsaicin compound that obtains is made into the stock solution that capsaicin compound concentration is 85 grams per liter with acetonitrile, with n-hexane / ethyl acetate binary mixed solvent (wherein acetic acid The molar fraction of ethyl ester is 5%) as extractant, with acetonitrile as washing agent, the flow ratio between raw material liquid, extractant, washing agent three is 2.6: 27: 1, at 45 ℃ figure 1 Fractional extraction is carried out in the fractionation extraction device shown (16 stages in extraction section and 8 stages in washing section), the raffinate is collected, water and organic solvent...

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Abstract

The invention discloses a method for separating capsaicinoids monomers from capsaicinoids compounds. According to the method, polar organic solvents are used as solvents, binary mixed solvents formed by weak polar organic solvents and middle-grade polar organic solvents are used as extracting agents; or polar organic solvent water solution is used as solvents, weak polar organic solvents are used as extracting agents, a fractionation extraction method is adopted for efficiently separating the capsaicinoids monomers from the capsaicinoids compounds containing capsaicinoids, dihydro capsaicinoids and the like. The method has the advantages that the separation efficiency is high, the solvent consumption is small, safety and environment protection are realized, the industrial production is easy, and the like.

Description

technical field [0001] The invention relates to a method for separating capsaicin monomers, belonging to the technical field of chemical engineering, in particular to a method for separating capsaicin monomers from capsaicin compounds. Background technique [0002] Natural capsaicin compounds are a class of extremely pungent vanilla amide alkaloids isolated from the pepper fruit of the Solanaceae plant. Studies have shown that capsaicin compounds have antibacterial, analgesic, antihypertensive, blood fat-lowering, and appetite-stimulating properties. In addition, it is widely used in food industry, military ammunition, pest control and so on. [0003] The main components of capsaicin compounds are capsaicin and dihydrocapsaicin, and the total mass fraction of the two can reach more than 90%. In addition, there are more than ten kinds of substances such as nordihydrocapsaicin, homodihydrocapsaicin and homocapsaicin. . Capsaicin is the main active ingredient of capsaicin com...

Claims

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Application Information

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IPC IPC(8): C07C233/20C07C231/24
Inventor 邢华斌曹义风任其龙杨启炜苏宝根鲍宗必杨亦文何芷琪苏云
Owner ZHEJIANG UNIV
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