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Method for extracting isothiocyanate high-purity product from brassicaceous vegetable seeds

A technology of cruciferous vegetables and isothiocyanates, which is applied in fermentation and other directions, can solve the problems of limited extraction or separation and purification of isothiocyanates, experimental research on the effect of isothiocyanates, large consumption of raw materials for processing, low purity, etc., to achieve improved Effects of high-value utilization efficiency, efficiency improvement, and low solution rate

Inactive Publication Date: 2018-05-04
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the extraction methods of isothiocyanate mainly include pressing method, steam distillation method, ultrasonic or microwave-assisted extraction method, enzyme-assisted extraction method, etc., and the separation and purification methods mainly include solvent extraction method, supercritical fluid extraction method, large-scale Pore ​​resin adsorption method, low-pressure silica gel column chromatography, high-speed countercurrent chromatography, etc., but these methods are mostly limited to the experimental research on the effect of a single technology and process on the extraction or separation and purification of isothiocyanates. Compared with its material composition, the content of glucosinolates in organs (including seeds) is generally less than 1%, and there are significant differences due to different vegetable varieties, growth environments, planting techniques and picking parts, making different extraction and preparation In the thiocyanate process, there are technical bottlenecks such as low yield, low purity, and large consumption of processing raw materials. For example, the Chinese published patent application CN1405316A, the crude isothiocyanate extract prepared by extraction cannot meet the requirements of the development of functional end products. Quality requirements, as well as the general public's market demand for isothiocyanate functional end products, establishing a method suitable for factory-scale production of high-purity isothiocyanate has become an urgent task in this field

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take fresh mature mustard seeds, add 0.8 times the weight of deionized water, grind into a slurry, then use a mixture of citric acid and Vc with a mass ratio of 2:1 to adjust the pH to 5.5, seal it with a plastic film, and ferment at 50 ° C for 20 hours , to obtain a fermentation slurry, add 1 times the volume of ethyl acetate to the fermentation slurry, extract twice under the conditions of shaking time 25 minutes, temperature 20°C, and standing extraction time 70 minutes, combine the extracts, and extract at -0.09MPa, 50 Concentrate under reduced pressure at ℃, recover ethyl acetate, and then vacuum freeze-dry the concentrated solution at -0.05MPa and -42℃ to obtain crude isothiocyanate extract; prepare the crude extract with deionized water to obtain a mass concentration For a 1.5% solution, first use a nano-membrane with a molecular weight cut-off of 2000Da to separate by nanofiltration at 35°C and 2.8MPa, and when the weight of the filtrate is 90% of the weight of t...

Embodiment 2

[0032] Take fresh mature mustard seeds, add 1.2 times the weight of deionized water, grind them into a slurry, then use a mixture of citric acid and Vc with a mass ratio of 2:1 to adjust the pH value to 6.5, seal with a plastic film, and ferment at 60°C 16h to obtain the fermentation slurry, add ethyl acetate 1.4 times the volume of the fermentation slurry to the fermentation slurry, extract twice at a shaking time of 35 minutes, a temperature of 30°C, and a standing extraction time of 50 minutes, combine the extracts, and extract at -0.05 Concentrate under reduced pressure at MPa and 60°C, recover ethyl acetate, then vacuum freeze-dry the concentrated solution at -0.09MPa, -38°C to obtain the crude extract of isothiocyanate; prepare the crude extract with deionized water To form a solution with a mass concentration of 2.5%, first use a nano-membrane with a molecular weight cut-off of 2000Da to perform nanofiltration separation at 40°C and 2.4MPa, and when the weight of the fil...

Embodiment 3

[0035] Take fresh mature broccoli seeds, add 1.0 times the weight of deionized water, grind it into a slurry, then adjust the pH value to 6.0 with a mixture of citric acid and Vc with a mass ratio of 2:1, seal it with a plastic film, and ferment at 55°C After 18 hours, the fermented slurry was obtained; the ethyl acetate of 1.2 times the volume of the fermented slurry was added to the fermented slurry, extracted twice at a shaking time of 30 minutes, a temperature of 25°C, and a static extraction time of 60 minutes, and the combined extracts were extracted at -0.07 Concentrate under reduced pressure at MPa and 55°C, recover ethyl acetate, vacuum freeze-dry the concentrate at -0.07MPa, -40°C to obtain crude isothiocyanate extract; deionize the crude extract with deionized water Prepare a solution with a mass concentration of 2.0%, and first use a nano-membrane with a molecular weight cut-off of 2000Da to conduct nanofiltration separation at 37.5°C and 2.6MPa, and when the weight...

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PUM

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Abstract

The invention discloses a method extracting an isothiocyanate high-purity product from brassicaceous vegetable seeds. According to the method, fresh mature brassicaceous vegetable seeds which containrice resources and have a high glucosinolate content are utilized as a raw material. The method comprises the steps: firstly, adding water into the raw material, grinding the raw material into slurryand performing fermentation treatment; then sequentially utilizing advanced extracting technologies of ethyl acetate extraction, nanofilm preliminary purification, polyamide resin purification, HP2MGLresin secondary purification, crystallization and the like to take technical breakthrough in factory scale production of the isothiocyanate high-purity product and obtain high-purity isothiocyanate extract. Not only is the excellent raw material is provided for researching pharmacological action and drug efficacy and developing a functional terminal production, but also safe, convenient, reasonable and economical high-valued utilization of the brassicaceous vegetable seed resources is really achieved, and a green chemical production idea and a cyclic economy strategy are fully expressed.

Description

technical field [0001] The invention relates to a method for extracting high-purity isothiocyanate from cruciferous vegetable seeds, especially a method of firstly adding water to grind the raw material into a slurry and performing fermentation treatment, followed by ethyl acetate extraction and nano-membrane preliminary Purification, polyamide resin purification, HP2MGL resin re-purification, crystallization and other extraction processes to prepare high-purity isothiocyanate. Background technique [0002] Glucosinolates are an important class of secondary metabolites in plants. Isothiocyanate is the enzymatic hydrolysis product of glucosinolate, which is widely and abundantly present in cruciferous vegetable plants, under the action of its myrosinase. Studies have shown that the content of glucosinolate and myrosinase in mature mustard, broccoli and other vegetable seeds is high, but in normal vegetable plant tissues, glucosinolate and myrosinase exist independently of ea...

Claims

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Application Information

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IPC IPC(8): C12P13/00
CPCC12P13/00
Inventor 肖文军邵元元彭影琦刘安
Owner HUNAN AGRICULTURAL UNIV
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