Production of high-purity capsaicin crystal by ion exchange resin method

The technology of ion exchange resin and crystal is applied in the field of producing high-purity capsaicin crystal, can solve the problems of low extraction rate, high investment cost, low degree of industrialization and the like, and achieves the effect of strong adsorption

Inactive Publication Date: 2007-10-24
陕西中青旅正达科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of this invention is to provide a kind of method that produces capsaicin compound crystal with ion-exchange resin method, to overcome the shortcoming that the processing route that existing technology exists is long, industrialization degree is not high, investment cost is high and extraction rate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] (1) extraction: take by weighing capsaicin essence 200g that contains capsaicin compound total content and be 6.2%, (1) after dissolving and filtering with 800ml n-hexane, the filtrate adds 85% ethanol of 800ml and separates after stirring 1h at 40°C,

[0024] (2) The n-hexane phase extract is extracted twice with ethanol according to the same method, and the ethanol phases are combined;

[0025] (2) adjust the pH value: adjust the ethanol phase pH=10.8 with 5% NaOH solution;

[0026] (3) Add the ethanol phase to the D290 anion exchange column at a flow rate of 1000ml / h, first wash it with 60% ethanol until the eluate is colorless, the amount of ethanol for washing the column is 9L, and then use 5% NaHSO 4 2L replacement resin, flow rate is 1500ml / h, in NaHSO 4 After the addition, stay for 20 minutes, then wash with deionized water at a flow rate of 4L / h until the effluent is free of SO 4 - ions, finally wash the column with 85% ethanol at a flow rate of 1L / h until ...

example 2

[0028] Example two: (1) extraction: take by weighing the capsicum resin 282g after Yunnan capsicum powder extracts red pigment, its capsaicin content is 4.5%, dissolve with 700ml sherwood oil, add 60% acetone solution 700ml to extract three times each time, merge acetone Mutually;

[0029] (2) Adjust the pH value: add NaOH to adjust the pH of the acetone phase to 10;

[0030] (3) Put on the column (the column type is D261), and wash with 50% alcohol solution until the acetone is colorless, release acetone, wash the column with 4L of water, and use 10% NaHSO 4 After replacing the resin, wash with deionized water until the effluent is free of SO 4 - ion. Elute the capsaicin compound with ethyl acetate until the capsaicin content of the eluate is less than 10ppm;

[0031](4) Concentrate in vacuum at 60° C. to make it crystallize, rinse with petroleum ether and then immerse and filter to obtain 11.68 g of crystalline capsaicin compounds with a total alkali content of 95.04%, a...

example 3

[0032] Example three: (1) extraction: take capsaicin compound total content and be 8.51% capsicum extract 200g, dissolve with 700ml sherwood oil and extract three times with 700ml of 78% ethanol, the ethanol extract merges;

[0033] (2) adjust pH value: adjust pH=10.5 with NaOH;

[0034] (3) Join in the anion-exchange column (D290) after filtration, and wash with 90% ethanol until the effluent is colorless, drain the ethanol and rinse the ion-exchange column with water, wash with 8% NaHSO 4 After replacement, wash with deionized water until the water is free of SO 4 - ion. Elute the exchange column with a mixed solvent of ethanol and ethyl acetate until the content of capsaicin compounds in the eluate is less than 10ppm;

[0035] (4) Evaporating the mixed solvent, washing and filtering with water and n-hexane respectively, and vacuum-drying at 40° C. to obtain 16.16 g of crystalline products with a total content of capsaicinoids of 95.4%, with a yield of 90.58%.

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Abstract

A process for preparing high-purity capsaicin crystal by ion exchange resin method includes such steps as providing the hot resin generated by extracting capic pigment or the hot pepper extract, extracting in non-polar solvent, extracting in polar solvent, regulating pH value, exchange adsorbing by resin column, eluting, vacuum distilling for removing organic solvent, washing, and cooling while crystallizing.

Description

Technical field: [0001] The invention relates to a method for producing high-purity capsaicin crystals by an ion exchange resin method. Background technique: [0002] The spicy ingredient in chili peppers is commonly known as capsaicin, and capsaicin crystals are widely used in food, medicine, paint, military, agriculture and many other fields in the form of products of different purity. At present, the production and extraction of capsaicin crystals can be basically divided into two types from the processing of source raw materials. The first is to directly extract capsaicin crystals through the extraction and refining process of chili powder; the second is to extract the spicy resin from chili peppers, or Commercially available capsicum extract (also known as capsicum resin) is extracted and refined to extract capsaicin crystals. The process of preparing capsaicin crystals from these two raw materials adopts two steps of crude extraction, purification and recrystallizatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/18B01D15/04B01D11/02A23L27/10
Inventor 邵纪生陈开勋陈国亮梁建中梁朝阳
Owner 陕西中青旅正达科技发展有限公司
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