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Preparation of capsicine

A technology of capsaicin and capsicum, which is applied in the preparation of carboxylic acid amide optical isomers, pharmaceutical formulations, and medical preparations containing active ingredients, etc., can solve the problems of low yield of capsaicin, fine crystallization, complicated extraction process, etc. problems, to achieve the effect of easy elution and regeneration, large sample loading, and simplified production process

Inactive Publication Date: 2008-11-05
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the problems of complex processes such as the existing extraction process, low yield of capsaicin, fine crystallization, etc., and the specific contents are as follows:

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 100g of properly crushed pepper, extract with 5% NaOH warm water for 12h, filter, add dilute hydrochloric acid to the filtrate to adjust the pH, control the flow rate, add the extract to the pretreated resin column, and use appropriate amount of water, ethanol with water or Aqueous acetone cleaning, flow rate 20mL min -1 . After elution with ethanol, the eluate was concentrated under reduced pressure and left to stand to precipitate capsaicin crystals, which were then dried to obtain 50 mg. The crystallization was detected by HPLC, with capsaicin as the reference substance, the content of capsaicin was 92.0%.

Embodiment 2

[0019] Weigh 100g of properly crushed pepper, extract with 5% NaOH warm water for 12h, filter, add dilute hydrochloric acid to the filtrate to adjust the pH, control the flow rate, add the extract to the pretreated resin column, and use appropriate amount of water, ethanol with water or Aqueous acetone cleaning, flow rate 20mL min -1 . After elution with ethanol, the eluate was concentrated under reduced pressure and left to stand to precipitate capsaicin crystals, which were then dried to obtain 52 mg. The crystallization was detected by HPLC, with capsaicin as the reference substance, the content of capsaicin was 95.6%.

Embodiment 3

[0021] HPLC detection of capsaicin

[0022] 1. Instruments, reagents and medicines:

[0023] SHIMADZU high-performance liquid chromatography (LC-10AT pump, LC-10 UV detector) (Japan), N2000 chromatography workstation (Institute of Intelligent Information Engineering, Zhejiang University). Capsaicin (capsaicin) was purchased from Sigma (purity>95%).

[0024] 2. Chromatographic conditions

[0025] Column: Kromasil C 18 (250mm×4.6mm, 5μm); mobile phase: methanol-water (65:35, containing 0.1% phosphoric acid); flow rate 1.0mL min -1 ; The detection wavelength is 345nm, and the injection volume is 20μl.

[0026] 3. Sample determination

[0027] Reference substance solution: Weigh an appropriate amount of capsaicin reference substance, accurately weigh it, put it in a 2mL volumetric flask, dissolve it in methanol, and dilute to the mark to make 0.04mg·mL -1 capsaicin reference solution.

[0028] Test solution: Weigh 4.0 mg of capsaicin, accurately weighed, put in a 10 mL volu...

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PUM

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Abstract

The invention discloses a method for preparing capsicine by adopting styrene macroporous resin. Compared with the technique disclosed by the existing invention and literature report, the method has the advantages of not using a large quantity of organic solvents, needing no special devices, large absorption amount of the absorption materials and being easy to regenerate, etc.; the method relates to a novel technique which is environment friendly for separating and refining capsicine from pepper. The method takes proper cracked peppers as the raw material and adopts alkaline water to extract; an extraction liquid is filtered or centrifugally deposited; flow speed is controlled to add the extraction liquid to a pre-processed resin column and then proper water and hydrous ethanol or hydrous acetone is used for washing in sequence; a single organic solvent is used for eluting; then an eluting liquid is decompressed, condensed and deposited, the capsicine crystallization is separated out and then the capsicine is obtained by drying. By taking the capsicine as a comparison product, the capsicine content of the crystallization detected by HPLC is more than 90 percent.

Description

technical field [0001] The invention relates to a method for extracting and separating active ingredients of natural products, in particular to a method for extracting and separating capsaicin from capsicum. Background technique [0002] Capsaicin has high medicinal value and economic value, and is widely used in medicine, light chemical, food industry and military fields. The method for extracting capsaicin from natural capsicum is generally based on its solubility characteristics, leaching with organic solvents and chromatographic separation, and crystallizing through organic solvents at low temperatures. At present, the commonly used extraction method has alkaline water extraction method (Zhao Aiyun, et al. Extraction technology of capsaicin in capsicum essence [J]. Food and Fermentation Industry, 2003, 28 (7): 82-83. Luo Chunli, etc. acid-base - Discussion on preparation of capsaicin compounds by extraction method [J]. Food Industry Science and Technology, 2007, 28 (5):...

Claims

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Application Information

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IPC IPC(8): C07C233/17C07C231/16A61K36/81
Inventor 魏英勤崔波马烽袁传贞班青
Owner QILU UNIV OF TECH
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