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Method of preparing capsaicine

A technology for capsaicin and capsaicin, which is applied in the field of preparation of capsaicin, can solve the problems of high production environment and equipment requirements, complicated extraction process, unfavorable industrialized production and the like, and achieves low equipment requirements, no environmental pollution, good quality The effect of adsorption

Active Publication Date: 2015-04-22
SHANDONG LUYE PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The extraction process is complex and cumbersome, and adopting aluminum oxide to carry out column chromatography can produce significant adsorption to capsaicin, resulting in the loss of capsaicin;
[0006] (2) Use diethyl ether and petroleum ether reagents in the crystallization process, and carry out centrifugation to the crystallization product at the same time. This method is very easy to explode during operation, and the vaporized solvent produced by centrifugation will produce a strong pungent smell, so The production environment and equipment are very demanding, which will pollute the environment and is not conducive to industrial production

Method used

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  • Method of preparing capsaicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take capsicum essence 0.3kg and transfer to a separatory funnel, add 1.5L of ethyl acetate to dissolve it, add 75g of sodium carbonate and 15g of sodium chloride into 1.5L of purified water to dissolve the prepared mixed lye for extraction, let stand for 12 hours, the ethyl acetate layer was concentrated and evaporated to dryness to obtain an extract oil.

[0023] The extracted oil was dissolved in 50% ethanol and subjected to polyamide column chromatography with 50% ethanol as the eluent. The eluate rich in capsaicin was collected, concentrated, and evaporated to dryness to obtain column chromatography oil.

[0024] The column chromatography oil was weighed, dissolved with 0.4 times the weight of the column chromatography oil and n-hexane-ethyl acetate with a volume ratio of 20:80, transferred to a -10°C freezer for 24 hours, and suction filtered to obtain the needle crystalline product. The content of capsaicin detected by HPLC is 94.9%, and the transfer rate of caps...

Embodiment 2

[0026] Take capsicum essence 0.5kg and transfer to a separatory funnel, add ethyl acetate 2.5L to make it dissolve, add 125g sodium carbonate and 25g sodium chloride to 2.5L purified water and dissolve the mixed lye prepared for extraction, let stand for 12 hours, the ethyl acetate layer was concentrated and evaporated to dryness to obtain an extract oil.

[0027] The extracted oil was dissolved in 60% ethanol and subjected to polyamide column chromatography with 60% ethanol as the eluent. The eluate rich in capsaicin was collected, concentrated, and evaporated to dryness to obtain column chromatography oil.

[0028] The column chromatography oil was weighed, dissolved with 0.4 times the weight of the column chromatography oil and n-hexane-ethyl acetate with a volume ratio of 30:70, transferred to a -12°C freezer for 24 hours, and suction filtered to obtain the needle crystalline product. The content of capsaicin detected by HPLC is 93.5%, and the transfer rate of capsaicin i...

Embodiment 3

[0030] Weigh 1 kg of capsicum essence and transfer it to a multifunctional glass reaction kettle, add 5 L of ethyl acetate to dissolve it, add 300 g of sodium carbonate and 50 g of sodium chloride to 5 L of purified water to dissolve the mixed lye for extraction, and let it stand for 12 hours , the ethyl acetate layer was concentrated and evaporated to dryness to obtain an extract oil.

[0031] The extracted oil was dissolved in 60% ethanol and subjected to polyamide column chromatography with 60% ethanol as the eluent. The eluate rich in capsaicin was collected, concentrated, and evaporated to dryness to obtain column chromatography oil.

[0032] The column chromatography oil was weighed, dissolved in n-hexane-ethyl acetate with a volume ratio of 40:60 and 1 times the weight of the column chromatography oil, transferred to a -15°C freezer for 30 hours, and suction filtered to obtain the needle crystalline product. The content of capsaicin detected by HPLC is 95.2%, and the t...

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Abstract

The invention provides a preparing method for capsaicine, which comprises the following steps: chilli extract is sequentially subjected to extraction, column chromatography, crystallization and filtration; and the column chromatography is the polyamide column chromatography, and an obtained column chromatography oily substance is dissolved in one of solutions, such as the mixture of cyclohexane and vinegar naphtha, the mixture of normal hexane and the vinegar naphtha , the mixture of the normal heptane and the vinegar naphtha, the mixture of ligarine and the vinegar naphtha, acetone or alcohol, and then is subjected to crystallization and filtration, thereby obtaining the capsaicine crystal.

Description

technical field [0001] The invention relates to a preparation method of capsaicin. Background technique [0002] Capsaicin is the main component of hot pepper components. High-purity capsaicin has many physiological activities and can be used in medicine, such as analgesia, treatment of skin diseases and arthritis, etc.; it can be used in biochemical pesticides to effectively expel aphids, leaf-eating Insects, etc.; can also be used in diet food. In addition, capsaicin can also be used to produce functional coatings, which can be applied to the surface of cables and wood to prevent rats from biting, and can also be used as raw materials for making tear gas bombs and defensive weapons. Because capsaicin has such a wide range of uses, the research on its preparation method has also been paid more and more attention by people. [0003] At present, the methods for preparing capsaicin mainly include solvent extraction, molecular distillation, ion exchange, column chromatography...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/20C07C231/24
Inventor 姜永涛白景李菊阮征于娟徐光
Owner SHANDONG LUYE PHARMA CO LTD