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Method for purifying capsicine compound from capsicol resin by using ammoniacal liquor

A technology for capsicum oleoresin and capsaicin, which is applied in the field of extraction of capsaicinoid compounds, can solve the problems of difficult recycling of alkali metal salts, increase the burden of waste liquid treatment, unfavorable purification steps, etc., and achieves easy large-scale production and production cost. Low, inexpensive effect

Inactive Publication Date: 2007-10-31
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem that this method exists is: alkali concentration is high, intensity is big, operation risk is high; The alkali metal salt that generates after acidification is difficult to recycle, causes great waste; Capsicum oleoresin lye solution viscosity is high, easily forms jelly shape, a stubborn emulsified layer that is easy to form during extraction, which is not conducive to the subsequent purification steps
Yang Depo, Yao Baoshu, etc. applied molecular distillation (CN1392136A, CN200510013075.4) to partially solve the problem of emulsification, but added more salt substances, which increased the burden of waste liquid treatment

Method used

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  • Method for purifying capsicine compound from capsicol resin by using ammoniacal liquor

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Embodiment 1

[0024] Get capsaicin content and account for 0.5% capsicum oleoresin 2g of gross weight, add 50ml 25% concentrated ammonia water, react in autoclave, the pressure in autoclave is 13.5atm, and temperature is 90 ℃, and reaction time 10min. The extract was distilled at 70°C. The distilled extract was titrated with hydrochloric acid to pH=4, extracted with 50 ml of n-hexane, centrifuged for 5 min to separate the organic phase, concentrated under reduced pressure to recover n-hexane to obtain a concentrated solution. Add 10ml of diethyl ether to the concentrated solution, freeze and crystallize at -10°C, and obtain 13.8 mg of capsaicin compound crystals, which are detected by high performance liquid chromatography and contain: 52.8% capsaicin, 38.2% dihydrocapsaicin, and 38.2% capsaicin nordihydrocapsaicin Alkali 6%. It can be seen that the content of the obtained capsaicin is: 7.29mg, and its yield is: 72.9%.

Embodiment 2

[0026] Get capsaicin content and account for the capsicum oleoresin 2g of gross weight 0.5%, add 30ml 25% concentrated ammonia water, react in autoclave, the pressure in autoclave is 5atm, and temperature is 70 ℃, and reaction times 1 hour. The extract was distilled at 70°C. The extract after the ammonia gas was evaporated was titrated with hydrochloric acid to pH = 7, extracted twice with 50 ml of n-hexane, left to stand for 0.5 hour, concentrated under reduced pressure to recover n-hexane to obtain a concentrated solution. Add 10ml of diethyl ether to the concentrated solution, freeze and crystallize at -10°C, and obtain 15.1 mg of capsaicin compound crystals. After detection by high performance liquid chromatography, the obtained crystals contain: capsaicin 51.4%, dihydrocapsaicin 37.3%, nordihydrocapsaicin Capsaicin 7.1%. It can be seen that the content of the obtained capsaicin is: 7.25mg, and its yield is: 72.5%.

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Abstract

The invention discloses an extracting method of capsicine compound, which comprises the following steps: choosing capsicol resin as raw material; dissolving into ammonia water; reacting in autoclave under high temperature; extracting capsicine; distilling extract; reclaiming ammonia; acidifying; extracting organic solvent; concentrating; cooling; crystallizing; getting the product. This invention possesses simple production method, low cost and high quality, which can replace alkali metal hydroxide purifying method to produce capsicine compound.

Description

technical field [0001] The invention belongs to a method for extracting capsaicin compounds, in particular to a method for purifying capsaicin compounds from capsicum oleoresin with ammonia water. technical background [0002] Capsaicinoids are substances that make chili peppers taste spicy. At present, more than 15 kinds of capsaicinoids (capsaicinoids) compounds have been identified from natural products, all of which are vanillyl amino and E-C 8 ~C 13 Alkenoic or alkanoic acid combination products. The most important of these are Capsaicin, Dihydrocapsaicin and Nordihydrocapsaicin. [0003] Capsaicin compounds have important application value in various fields such as medicine, military affairs, pesticides, coatings and so on. The application of capsaicinoid compounds in the field of medicine has attracted people's attention especially. It is clinically used to treat rheumatoid arthritis and osteoarthritis, neuropathic pain. In recent years, researchers have used ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C231/12C07C233/17
Inventor 雷超常志东刘会洲安震涛李燕青刘吉李斌马印臣
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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