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A kind of preparation method of high-purity capsaicin

A capsaicin and high-purity technology, which is applied in the separation/purification of carboxylic acid amide, bulk chemical production, organic chemistry, etc., can solve the problems of large solvent consumption, low product yield, and difficulty in industrialized production, and achieve non-spicy The effect of low loss and simple process operation

Active Publication Date: 2017-04-19
CHENGUANG BIOTECH GRP HANDAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Patent CN103254092 A and patent CN102432489B respectively adopt the method of high-efficiency liquid phase and self-made reversed-phase chromatographic column to separate crude capsaicin and obtain monomers such as high-purity capsaicin and dihydrocapsaicin. The process equipment and steps are complicated, and the solvent Large dosage, it is difficult to realize industrial production
[0006] In the existing high-purity capsaicin preparation process, most of them are difficult to realize industrialized production, and all have the shortcomings of large solvent consumption, low product yield and high production cost, and its output is not enough to supply demand. Therefore, the preparation of high-purity capsicum Alkali production technology research has huge economic benefits

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 10kg of capsicum oleoresin with a spiciness of 20%, add 3kg of sodium hydroxide solution with a concentration of 20wt%, and stir continuously at 60°C for 3h for saponification. The saponified liquid is subjected to supercritical extraction, the primary extraction pressure is 10MPa, the extraction temperature is 40°C, and the extraction time is 3h. After the primary extraction is completed, release the isolate, continue to increase the pressure of the extraction kettle to 30Mpa, the extraction temperature is 55°C, and the extraction time is 6h. In the extraction kettle, a high-spicy capsicum oleoresin with a spicy degree of 81% is obtained. Obtain decolorized capsicum extract. Add high-spicy capsicum oleoresin into a 75% methanol solution equivalent to 5 times its weight, stir at 50°C for 30 minutes, cool down to 0°C after 0.5h, crystallize for 10h, and filter and separate to obtain capsaicin crystals 1.5 kg, the product purity is 98.1%, and the hotness yield is 73...

Embodiment 2

[0024] Take 10kg of capsicum oleoresin with a spicy degree of 30%, add 1kg of sodium hydroxide solution with a concentration of 20wt%, and stir continuously at 70°C for 2h for saponification. The saponification liquid is subjected to supercritical extraction, the primary extraction pressure is 15Mpa, the extraction temperature is 30°C, and the extraction time is 3h. After the primary extraction is completed, release the isolate, continue to increase the pressure of the extraction kettle to 25Mpa, the extraction temperature is 60°C, and the extraction time is 10h. In the extraction kettle, a high-spicy capsicum oleoresin with a spiciness of 85% is obtained. Obtain decolorized capsicum extract. Add high-spicy capsicum oleoresin into an 80% ethanol solution equivalent to twice its weight, stir at 40°C for 30 minutes, cool down to -10°C after 1 hour, crystallize for 5 hours, and separate by filtration to obtain capsaicin crystals 2.3 kg, the product purity is 98.0%, and the hotne...

Embodiment 3

[0026] Take 10kg of capsicum oleoresin with a spiciness of 20%, add 1.5kg of a sodium hydroxide solution with a concentration of 20wt%, and stir continuously at 68°C for 2.5h for saponification. The saponified liquid is subjected to supercritical extraction, the primary extraction pressure is 12Mpa, the extraction temperature is 33°C, and the extraction time is 3h. After the primary extraction is completed, release the isolate, continue to increase the pressure of the extraction kettle to 28Mpa, the extraction temperature is 56°C, the extraction time is 8h, and the high-spicy capsicum oleoresin with a spiciness of 82% is obtained in the extraction kettle. Obtain decolorized capsicum extract. Add high-spicy capsicum oleoresin into a 76% methanol solution equivalent to three times its weight, stir at 42°C for 30 minutes, cool down to -5°C after 0.5h, crystallize for 6h, and filter and separate to obtain capsaicin crystals 1.5kg, product purity 98.3%, spicy yield 73.7%.

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Abstract

The invention relates to a method for preparing high-purity capsaicin and belongs to the field of refining of natural products. According to the method, a low-pungency degree capsicum oleoresin is taken as a raw material, and the high-purity natural capsaicin is prepared by combining supercritical CO2 extraction and a crystallization technology. The purity of the obtained capsaicin crystal is more than 98 percent, and the pungency degree yield of the product is more than 70 percent. The supercritical secondary extraction isolate can be directly used as decolorized oleoresin capsicum, and the pungency degree loss is basically avoided. The method is easy to operate, and the continuous industrial production is easily realized.

Description

technical field [0001] The invention belongs to the technical field of refining natural products, and in particular relates to a preparation method of high-purity capsaicin. Background technique [0002] Natural capsaicin is a natural vanilla amide alkaloid prepared from capsicum oleoresin extracted from red peppers. The main components are capsaicin, dihydrocapsaicin and nordihydrocapsaicin. Capsaicin has physiological activity and long-lasting strong anti-inflammatory and analgesic effects, and has been widely used as an additive in the food and chemical industries and as an analgesic in the pharmaceutical industry. [0003] Patent CN100540528C discloses a method for preparing capsaicin based on low-spicy capsicum essence. First, ethyl acetate is added to the raw material to extract medium-spicy pepper essence, and then methanol is added to medium-spicy pepper essence to produce oily capsicum. Alkali mixture, finally using column chromatography and crystallization in sequ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/20C07C231/24
CPCY02P20/54
Inventor 齐立军褚延伟黄利勇魏占姣
Owner CHENGUANG BIOTECH GRP HANDAN CO LTD
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