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Method for extracting and separating glucoraphanin from broccoli seeds

A technology of broccoli seeds and glucoraphanin, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as low yield, small scale of preparation chromatography, and less product volume, and achieve simple process Ease of operation, cheap process and easy industrialization

Active Publication Date: 2016-05-11
PIONEER HERB IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in patent CN103709211, cauliflower is used as raw material to extract and separate glucoraphanin. After the primary separation with a weakly polar macroporous resin, high-purity glucoraphanin is obtained by separation with a silica gel column again. However, the content of the raw material glucoraphanin is relatively low. Large volume, difficult to store and transport, so the yield is low
Patent CN102295667 obtains high-purity glucoraphanin after multiple extractions and preparative chromatographic column separation, but the scale of preparative chromatographic analysis is small, and the amount of product obtained at a single time is small, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for extracting and isolating glucoraphanin from broccoli seeds, comprising the following steps:

[0026] (1) Take 200 g of dried broccoli seeds, treat them in an oven at 105°C for 30 minutes, then crush them, add 1000 mL of ethanol solution with a content of 65% (volume fraction), heat to 60°C for extraction for 1 hour, and filter to obtain a glucoraphanin solution. The glucoraphanin solution was concentrated in a rotary evaporator to 100 mL.

[0027] (2) Fill the column with the pretreated DM-301 macroporous adsorption resin, and the glucoraphanin concentrate passes through the resin column at a speed of 3BV / h, then washes with 4BV of deionized water, and then uses 4BV with a volume content of 95% ethanol solution for elution.

[0028] (3) The glucoraphanin eluate was concentrated in a rotary evaporator to 20 mL, mixed with 20 g of silica gel (300 mesh), and the solvent was evaporated to obtain silica gel for adsorbing glucoraphanin.

[0029] (4) Take 150g o...

Embodiment 2

[0033] A method for extracting and isolating glucoraphanin from broccoli seeds, comprising the following steps:

[0034] (1) Take 200g of dried broccoli seeds, treat them in an oven at 105°C for 30min, then crush them, add 1000mL of 65% ethanol solution, heat to 60°C for extraction for 1h, and filter to obtain a glucoraphanin solution. The glucoraphanin solution was concentrated in a rotary evaporator to 100 mL.

[0035] (2) The ADS-17 macroporous adsorption resin that has been pretreated is packed into the column, and the glucoraphanin concentrate passes through the resin column at a speed of 3BV / h, then washed with 4BV of deionized water, and then the content of 4BV volume is 95% ethanol solution for elution.

[0036] (3) The glucoraphanin eluate was concentrated in a rotary evaporator to 20 mL, mixed with 20 g of silica gel (300 mesh), and the solvent was evaporated to obtain silica gel for adsorbing glucoraphanin.

[0037] (4) Take 150g of silica gel (300 mesh), wet it w...

Embodiment 3

[0041] A method for extracting and isolating glucoraphanin from broccoli seeds, comprising the following steps:

[0042] (1) Take 200g of dried broccoli seeds and place them in an oven at 105°C for 20min, crush them, add 400mL of ethanol solution, heat to 40°C for extraction for 2h, filter, the filtrate is glucoraphanin solution, and the obtained sulforaphane The glucoraphanin solution is concentrated in a rotary evaporator until the volume is 1 / 3 of the volume of the original glucoraphanin solution to obtain a glucoraphanin concentrated solution;

[0043] (2) Fill the column with the pretreated ADS-17 macroporous adsorption resin, pass the glucoraphanin concentrate obtained in step (1) through the resin column at a speed of 1BV / h, and adsorb with the macroporous adsorption resin, wherein the The volume of the glucoraphanin concentrate of the column is 2BV;

[0044] (3) The macroporous adsorption resin adsorbing glucoraphanin is washed with deionized water, and then eluted wi...

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Abstract

The invention relates to a method for extracting and separating glucoraphanin from broccoli seeds. The method comprises the following steps that 1, a glucoraphanin solution is extracted from the broccoli seeds and concentrated to obtain a concentrated glucoraphanin solution; 2 the concentrated glucoraphanin solution is adsorbed through macroporous adsorption resin; 3, the macroporous adsorption resin is eluted with an ethanol solution to obtain resin eluate; 4, after the resin eluate is concentrated, silica gel is added, mixing is performed, ethanol is volatilized, and silica gel adsorbing glucoraphanin is obtained and added to the upper layer of a silica gel column obtained through silica gel column filling; 5, the silica gel column is eluted with eluent, eluate is collected, concentrated and dried, and then the glucoraphanin product is obtained. Compared with the prior art, the method has the advantages that the technology is simple and easy to operate, industrialization is easy, the macroporous resin and the silica gel are low in cost and easy to obtain, the whole technology is low in price and little in investment, and the high-purity glucoraphanin product can be obtained.

Description

technical field [0001] The invention relates to a method for purifying natural products, in particular to a method for extracting and separating glucoraphanin from broccoli seeds. Background technique [0002] Glucoraphanin (4-methylsulfinylbutenyl glucosinolate) widely exists in cruciferous plants, such as broccoli, kale, Brussels sprouts, cauliflower, horseradish, Chinese cabbage, etc. [Chinese Agricultural Science Bulletin, 2008, 24 (2): 335-338; Food Science and Technology, 2009, 34 (12): 250-252], among which active ingredients are the most in broccoli and cauliflower, especially the highest content in broccoli seeds. The degradation products of glucoraphanin are mainly sulforaphane, sulforaphane nitrile, and oxazolidinethione, among which sulforaphane has the highest content [Food Science and Technology, 2009, 34(12): 250-252]. Sulforaphane is a type of isothiocyanate with the strongest anti-cancer activity found in vegetables so far, and it is currently recognized as...

Claims

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Application Information

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IPC IPC(8): C07H15/14C07H1/08
CPCC07H1/08C07H15/14
Inventor 刘儒华刘锡建
Owner PIONEER HERB IND CO LTD
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