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Method for preparing sulforaphane

A technology of radish and radish, applied in the direction of organic chemistry, etc., can solve the problems of complex and cumbersome process, difficult to realize industrialization, and easy destruction of radish, so as to achieve increased content and purity, high selectivity, and high degree of industrialization Effect

Inactive Publication Date: 2011-11-09
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Because radishin is easily destroyed in high temperature or strong acid or strong alkali environment, the existing processes are complicated and cumbersome, and it is difficult to realize industrialization

Method used

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  • Method for preparing sulforaphane

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Experimental program
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Effect test

Embodiment 1

[0023] Grind radish seeds, take 20kg, add to the extraction tank, add 40kg of hydrochloric acid aqueous solution (pH5), heat to 50°C for 60 minutes, heat up to 80°C quickly, after 30 minutes, add 120kg of water, stir and extract for 2 hours, and filter out the liquid , add 100kg of water to extract, combine the two liquids, filter and add AB-8 macroporous resin for adsorption, wash neutral with water, take 6 times the amount of 50% ethanol solution to elute, collect the eluate, add hollow cellulose with a molecular weight cut-off of 400 Membrane nanofiltration, add appropriate amount of water for dialysis, collect the passing liquid and then add it to the reverse osmosis membrane to concentrate, collect the concentrated liquid and add an equal volume of dichloromethane to extract, extract 4 times, collect the extract to recover the reagent under reduced pressure, 9g oily rapatin, after The content detected by HPLC is 75.6%.

Embodiment 2

[0025] Grind radish seeds, take 20kg, add to the extraction tank, add 60kg of sulfuric acid aqueous solution (pH4), heat to 45°C for 60 minutes, then rapidly heat up to 80°C, after 30 minutes, add 100kg of water, stir and extract for 2 hours, and filter out the liquid , add 100kg of water to extract, combine the two liquids, filter and add D101 macroporous resin for adsorption, wash neutral with water, take 5 times the amount of 70% ethanol solution for elution, collect the eluate, add hollow cellulose membrane with a molecular weight cut-off of 500 Filtrate, add appropriate amount of water for dialysis, collect the passing liquid, add reverse osmosis membrane to concentrate, collect the concentrated liquid and add 2 times the volume of dichloromethane for extraction, extract 3 times, collect the extract and recover the reagent under reduced pressure, 11g oily rapatin, after high-efficiency The liquid detection content was 70.1%.

Embodiment 3

[0027] Grind radish seeds, take 20kg, add to the extraction tank, add 60kg of sulfuric acid aqueous solution (pH4), heat to 45°C for 60 minutes, heat up to 80°C quickly, after 30 minutes, add 100kg of water, stir and extract for 2 hours, and filter out the liquid , add 100kg of water to extract, combine the two liquids, filter and add HPD100 macroporous resin for adsorption, wash neutral with water, take 5 times the amount of 60% ethanol solution for elution, collect the eluate, add hollow cellulose membrane with a molecular weight cut-off of 400 Filtrate, add appropriate amount of water for dialysis, collect the passing liquid, add reverse osmosis membrane to concentrate, collect the concentrated liquid and add 2 times the volume of dichloromethane for extraction, extract 3 times, collect the extract and recover the reagent under reduced pressure, 6g oily rapatin, after high-efficiency The liquid detection content was 71.2%.

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Abstract

The invention belongs to the field of natural product separation and discloses a method for preparing sulforaphane, which comprises the following steps of: 1) crushing a radish seed medicinal material, adding water in an amount which is 2 to 3 times that of the crushed medicinal material, regulating the pH to be 4-5, performing enzymolysis at the temperature of between 45 and 50DEG C for 30 to 60 minutes, quickly heating to 80DEG C for deactivating enzymes, adding water in an amount of 5 to 6 times that of the solution, stirring, extracting, filtering out liquid, adding water in an amount which is 5 to 6 times that of the materials, extracting, mixing liquid in two times, and filtering to obtain extracting solution; 2) adsorbing the extracting solution by using macroporous resin, washing with water to reach neutrality, eluting by using 50- to 70 percent of ethanol solution in an amount which is 5 to 6 times that of the solution, collecting eluent, performing nanofiltration by using a nanofiltration membrane, and concentrating the passing liquid by using a reverse osmosis membrane to obtain concentrated solution; and 3) extracting the concentrated solution by using dichloromethane, and recovering reagents from extracting solution under reduced pressure to obtain the sulforaphane. The sulforaphane is prepared by using the macroporous resin and a membrane separation technology; and the process is easy to operate, the production cost is low and the method is suitable for industrial production.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, and in particular relates to a preparation method of ratin. Background technique: [0002] Raphain (1-isothiocyanate-4-methylsulfonylbutane), also known as sulforaphane and sulforaphane, is a kind of isoglucoside obtained by enzymatic hydrolysis or acid hydrolysis of glucose rapsidase. Thiocyanate, soluble in water, methanol and chloroform, easily soluble in ether, almost insoluble in petroleum ether, molecular weight 177.29, molecular formula C 6 h 11 S 2 NO, molecular structure formula: [0003] [0004] Raphanusin is liquid at room temperature, boiling point 125~130° / 0.015mm, [α]19 / D-107°(C=1.37, chloroform), [α]14 / D-136°(C=1.38, ethanol) . Talalay et al. proved that radhacetin has good anticancer activity on esophageal cancer, colon cancer, breast cancer, etc., which has aroused extensive attention of scholars from various countries on glucosinolate components of crucife...

Claims

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Application Information

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IPC IPC(8): C07C331/20
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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