High-purity capsaicin compound refining crystallization method

A technology of capsaicin and compounds, which is applied in the field of crystallization, can solve problems such as complex equipment and steps, difficulty in industrial production, and resin regeneration, and achieve the effects of low production cost, no discharge of three wastes, and short production cycle

Active Publication Date: 2012-06-27
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The equipment and steps of the resin method are complex, the amount of solvent used is large, and there is also the problem of resin regeneration, which makes it difficult to realize industrial production

Method used

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  • High-purity capsaicin compound refining crystallization method
  • High-purity capsaicin compound refining crystallization method
  • High-purity capsaicin compound refining crystallization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Crystallization to prepare high-purity natural capsaicin compound crystals:

[0019] Add 4.00 g of crude natural capsaicin compounds with a mass purity of 50% into a mixed solvent of 200 mL of petroleum ether and 800 mL of n-butyl ether, stir and dissolve at a constant temperature of 45 ° C, and filter after continuous stirring for 40 minutes; the filtrate is transferred to a crystallizer Inside, carry out cooling and crystallization under stirring, the stirring speed is 100r / min, after 6 hours, the temperature drops to 10°C; after the crystallization is complete, filter and separate, wash the crystals with a mixed solvent, and ventilate and dry the crystals at 55°C for 4 hours , to obtain white high-purity natural capsaicin compound crystal product 1.47g.

[0020] HPLC detection of total capsaicin content: 99.80%

[0021] HPLC detection capsaicin monomer content: 67.17%

[0022] The sum of the content of capsaicin monomer and dihydrocapsaicin detected by HPLC is 91.0...

Embodiment 2

[0025] Crystallization to prepare high-purity natural capsaicin compound crystals:

[0026] 25.00g mass purity is that 80% raw material natural capsaicin compound crude product is added in the mixed solvent of 2000mL sherwood oil and 500mL ethanol, stirs and dissolves under the constant temperature of 40 ℃, filters after continuous stirring 60 minutes; Filtrate moves in the crystallizer, Cool and crystallize under stirring, the stirring speed is 300r / min, and the temperature drops to -10°C after 10 hours; after the crystallization is complete, filter and separate, wash the crystals with a mixed solvent, and vacuum dry the crystals at 55°C for 3 hours. Obtained 15.58g of white high-purity natural capsaicin compound crystal product.

[0027] HPLC detection of total capsaicin content: 99.2%

[0028] HPLC detection capsaicin monomer content: 70.21%

[0029] The sum of the content of capsaicin monomer and dihydrocapsaicin detected by HPLC is 92.03%

[0030] Product quality yield...

Embodiment 3

[0032] Crystallization to prepare high-purity natural capsaicin compound crystals:

[0033] Add 2.96g of crude natural capsaicin compounds with a mass purity of 60% into a mixed solvent of 250mL of n-hexane and 250mL of isopropyl ether, stir and dissolve at a constant temperature of 60°C, and filter after continuous stirring for 10 minutes; the filtrate is transferred to a crystallizer Inside, carry out cooling crystallization under stirring, the stirring speed is 500r / min, and after 1 hour the temperature drops to 25°C; after the crystallization is complete, filter and separate, wash the crystals with a mixed solvent, and ventilate and dry the crystals at 45°C for 4.5 hours , to obtain white high-purity natural capsaicin compound crystal product 1.57g.

[0034] HPLC detection of total capsaicin content: 99.54%

[0035] HPLC detection capsaicin monomer content: 68.91%

[0036] The sum of the content of capsaicin monomer and dihydrocapsaicin detected by HPLC is 90.05%

[003...

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Abstract

The invention belongs to the technical field of crystallization, and discloses a high-purity capsaicin compound refining crystallization method. First, a raw material which is a capsaicin compound crude product with a mass concentration higher than 50% is added into a mixed solvent with a certain ratio, and is dissolved by stirring under a constant temperature; the solution is filtered, and is transferred into a crystallizing machine; the temperature of the solution is slowly reduced to -10 to 25 DEG C, and an operation time of a crystallization procedure is shorter than 10h; when crystallization is fully carried out, the mixture is filtered and dried, such that a white high-purity natural capsaicin compound crystal product is obtained. With the method, the obtained acicular capsaicin compound product crystals have crystal purity higher than 99% and crystal yield higher than 70%. With the method provided by the invention, quality and process yield of crystal products are greatly improved. The method is economic, practicable, and is characterized by short production period. The method is suitable for industrialized productions.

Description

technical field [0001] The invention belongs to the technical field of crystallization, in particular to a method for refining crystallization of high-purity capsaicin compounds (with a mass content of more than 99%). Specifically, it is a method for producing capsaicin compound crystals by adopting cooling crystallization technology. The needle-shaped capsaicin compound crystal obtained by the method has a purity of more than 99%, complete crystal habit, and is suitable for industrial production. Background technique [0002] Natural capsaicin compounds are spicy vanilla amide alkaloids contained in peppers, and their main components are capsaicin, dihydrocapsaicin and nordihydrocapsaicin, and the content of the three accounts for about 98%. Capsaicin compounds are widely used in important fields such as medicine, food, pesticides, military and coatings. It has a longer-lasting analgesic effect than morphine, can increase appetite, promote blood circulation and improve di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/20C07C233/18
Inventor 王静康闫浩王召侯宝红尹秋响张美景龚俊波王永莉鲍颖谢闯
Owner TIANJIN UNIV
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