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Method for preparing sulforaphen by virtue of subcritical fluid extraction

A subcritical fluid and sulforaphane technology, applied in the chemical industry, can solve the problems of restricting the development and utilization of sulforaphane, high raw material prices, poor thermal stability of sulforaphane, etc., achieve considerable economic benefits and social value, and improve conversion rate and content, the effect of no organic solvent residue

Inactive Publication Date: 2017-04-26
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing technology basically uses broccoli seeds as raw materials to extract sulforaphane, and the high price of raw materials greatly restricts the development and utilization of sulforaphane in terms of resources and costs
In addition, sulforaphane has poor thermal stability, separation and purification are difficult, and the conversion rate of extraction and preparation of sulforaphane by traditional methods is low, especially the problem of solvent residue in the process cannot be solved
while supercritical CO 2 The extremely high pressure operation above 25MPa required by the extraction method seriously restricts the industrial popularization and application of this technology

Method used

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  • Method for preparing sulforaphen by virtue of subcritical fluid extraction

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) Preparation of myrosinase: Take fresh cabbage, cool it to 3-5°C in the refrigerator, beat it with a homogenizer, add NaHCO with a pH of 7.5 to double the volume 3 Buffer solution, after filtering with 100-mesh double-layer gauze to obtain the filtrate, add 5 times the volume of ethanol of the filtrate to the filtrate at 3-5°C, mix evenly, and centrifuge under a high-speed refrigerated centrifuge (speed: 4000r / min, temperature: 4 -5°C), collected the precipitate and freeze-dried to obtain 53g of crude myrosinase, which was stored in a -20°C refrigerator for future use (for long-term storage, it should be stored in a -80°C refrigerator). (2) Enzymolysis reaction: Weigh 50.0kg of fresh broccoli stems and leaves, add 50.0kg of deionized water, homogenize with a homogenizer, adjust pH5.0-6.0 with 5% hydrochloric acid, according to 1000:1:0.8 (Materials: catalyst: crude myrosinase, (w / w / w) ratio is added to the catalyst and the crude myrosinase obtained in step 1, and the...

Embodiment 2

[0025] (1) Preparation of myrosinase: Take fresh cabbage, cool it to 3-5°C in the refrigerator, beat it with a homogenizer, add 1.5 times the volume of NaHCO with pH7.5 3 Buffer solution, after filtering with 100-mesh double-layer gauze to obtain the filtrate, add 6 times the volume of ethanol of the filtrate to the filtrate at 3-5°C, mix evenly, and centrifuge under a high-speed refrigerated centrifuge (speed: 5000r / min, temperature: 4 -5°C), collect and freeze-dry the precipitate to obtain 55 g of crude myrosinase, and put it in a -20°C refrigerator for frozen storage and standby (for long-term storage, it needs to be stored in a -80°C refrigerator). (2) Enzymolysis reaction: take by weighing 50.0kg of dried broccoli seeds, grind to 30-60 mesh, add 75.0kg deionized water, adjust pH5.0-6.0 with 5% hydrochloric acid, according to 1000:1.2:1.0 (raw material : Catalyst: myrosinase crude product, (w / w / w) ratio is added to the catalyst and the crude myrosinase obtained in step 1, ...

Embodiment 3

[0027] (1) Preparation of myrosinase: Take fresh cabbage, cool it to 3-5°C in the refrigerator, beat it with a homogenizer, add 0.8 times the volume of NaHCO with pH7.5 3 Buffer solution, after filtering with 100-mesh double-layer gauze to obtain the filtrate, add 4 times the volume of ethanol of the filtrate to the filtrate at 3-5°C, mix evenly, and centrifuge under a high-speed refrigerated centrifuge (speed: 5000r / min, temperature: 4 -5°C), collected the precipitate and freeze-dried to obtain 51 g of crude myrosinase, which was stored in a -20°C refrigerator for future use (for long-term storage, it should be stored in a -80°C refrigerator). (2) Enzymolysis reaction: take by weighing 50.0kg of fresh broccoli curd, add 50.0kg of deionized water, after homogenizing with a homogenizer, adjust pH5.0-6.0 with 5% hydrochloric acid, according to 1000:1:1 ( Raw materials: catalyst: crude myrosinase, (w / w / w) ratio is added to the catalyst and the crude myrosinase obtained in step 1,...

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Abstract

The invention discloses a method for preparing sulforaphen by virtue of subcritical fluid extraction. The method comprises the following steps: taking fresh cabbages, performing pulping, adding a buffer solution, mixing the materials uniformly, performing filtration, adding ethanol of which the volume dose is 5 times that of a filtrate into the filtrate, mixing the materials uniformly, and performing high-speed centrifugation to obtain a deposit namely a myrosin crude product; taking fresh brassica oleracea. L.var. italica plenck, adding deionized water, performing pulping, then adjusting the pH value of the mixture to be 5.0-6.0 by using 5% hydrochloric acid, adding a catalyst and the myrosin crude product with an added weight ratio of the brassica oleracea. L.var. italica plenck pulp to the catalyst to the myrosin crude product of 1000:1:0.8, and performing enzymolysis for 12h at 40-42 DEG C; adding a mixed solvent into a solid-liquid mixture after the enzymolysis, adding an entrainer, and performing subcritical fluid extraction for 60min; and collecting extract cut fractions to obtain an oily sulforaphen product. The method for preparing the sulforaphen, disclosed by the invention, greatly improves the conversion rate and the content of the sulforaphen in the brassica oleracea. L.var. italica plenck, reduces the production cost of the sulforaphen, and has very considerable economic benefits and social values.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, and more specifically relates to a method for preparing sulforaphane by subcritical fluid extraction. Background technique [0002] Sulforaphane (Sulforaphane), also known as "sulforaphane", only exists in cruciferous vegetables, and the content of broccoli (Brassica oleracea. L. var. italica Plenck) ranks first among all vegetables. Modern research shows that sulforaphane is one of the most powerful and effective new anticancer active ingredients among all the natural anticancer substances found so far. Biological activities such as anti-oxidation, anti-inflammation, whitening and freckle removal, and protection against ultraviolet radiation. In recent years, consumers in the field of cosmetics have greatly favored the "green factor" of pure natural herbal sources. Well-known domestic and foreign companies such as L'Oreal and Xiangyi Herbal have successively launched new products c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C331/22C12N9/24
CPCC07C331/22C12N9/24
Inventor 林海燕陈淼芳张盛黄科肖文军刘仲华
Owner HUNAN AGRICULTURAL UNIV
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