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New preparation method of 1-isothiocyanic acid-4-methanesulfonyl-(2-ene) butane

A technology of methanesulfonyl and isothiocyanate, applied in the field of biochemistry, can solve the problems of immobilization, difficult operation, low product purity, etc., and achieves the effects of mild reaction conditions, increased reaction probability, and easy popularization and application.

Inactive Publication Date: 2014-11-19
重庆海巨农业发展有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems in this method are: 1. The seeds are not degreased. Due to the blocking of oil, the sinaprin and glucuronidase in the broccoli seeds are difficult to effectively contact, resulting in a low production rate of sulforaphane; 2. Immobilization of the extracted myrosinase, the free enzyme has a short half-life and is easily inactivated; 3. The organic solvent used - acetone has a strong ability to denature the enzyme protein, resulting in a large amount of denaturation and inactivation of the myrosinase; 4 .Vacuum drying at a higher temperature, sulforaphane is unstable, easy to rearrange to form a variety of isomers, and the product purity is low
The main problems of this method are: ① supercritical CO 2 The degreasing effect is poor, only 1 / 3 of the oil in the radish seeds can be removed, and most of the oil remains in the defatted radish seed meal, hindering the release of glucosinolates and glucosinosidases, affecting the hydrolysis efficiency and product quality; and supercritical CO 2 The equipment investment is large, the device is complicated, and the operation is difficult; ②CO 2 It is difficult to fully recover the entraining agent and methanol-water eluent, etc., and the production cost is high; only the radish seeds are crushed, and the glucosinolates and glucosinosidases present in the cells are not recovered. Fully released, during the hydrolysis reaction, the diffusion rate is slow, and the amount of diffusion is limited, resulting in an increase in the hydrolysis reaction time, and a relative hydrolysis efficiency is reduced; ③The glucosinolate content in radish seeds is less, and the No added glucosinolate, so the yield of sulforaphane obtained by hydrolysis is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A method for preparing 1-isothiocyanate-4-methylsulfonyl-(2-ene)butane, the specific steps are as follows. 1. Preparation of radish seed crushing liquid

[0036] Take air-dried radish seeds with a moisture content lower than 4% respectively, disperse the air-dried radish seeds in ice water with the ratio of radish seed mass: ice-water volume ratio of 1kg: 1L, and discharge them in a rotary vane pulverizer under stirring smash. After the crushing is completed, the crushing liquid is collected to obtain the radish seed crushing liquid, which is used to prepare the degreasing fine grinding liquid.

[0037] 2. Preparation of enzyme-inactivated broccoli or rapeseed dispersion

[0038] Take broccoli seeds or rapeseeds, first crush them with a traditional Chinese medicine grinder, and then sieve them with a 20-mesh stainless steel sieve, and collect the sieved and unsifted materials respectively. For unscreened broccoli seed powder or rapeseed, return to the crusher for re-...

Embodiment 2

[0054] A method for preparing 1-isothiocyanate-4-methylsulfonyl-(2-ene)butane, the specific steps are as follows.

[0055] 1. Preparation of radish seed crushing liquid

[0056] Take air-dried radish seeds with a moisture content lower than 4% respectively, disperse the air-dried radish seeds in ice water at a ratio of 1 kg: 3 L of radish seed mass: ice-water volume ratio, and discharge them in a rotary vane pulverizer under stirring smash. After the crushing is completed, the crushing liquid is collected to obtain the radish seed crushing liquid, which is used to prepare the degreasing fine grinding liquid.

[0057] 2. Preparation of enzyme-inactivated broccoli or rapeseed dispersion

[0058] Take broccoli seeds or rapeseed, first crush them with a traditional Chinese medicine grinder, and then sieve them with a 40-mesh stainless steel sieve, and collect the sieved and unsifted materials respectively. For unscreened broccoli seed powder or rapeseed, return to the crusher f...

Embodiment 3

[0074] A method for preparing 1-isothiocyanate-4-methylsulfonyl-(2-ene)butane, the specific steps are as follows.

[0075] 1. Preparation of radish seed crushing liquid

[0076] Take the air-dried radish seeds with a moisture content lower than 4% respectively, disperse the air-dried radish seeds in ice water at a ratio of 1 kg: 5 L of the mass of radish seeds: the volume of ice water, and discharge them in a rotary vane pulverizer under stirring smash. After the crushing is completed, the crushing liquid is collected to obtain the radish seed crushing liquid, which is used to prepare the degreasing fine grinding liquid.

[0077] 2. Preparation of enzyme-inactivated broccoli or rapeseed dispersion

[0078] Take broccoli seeds or rapeseed, first crush them with a traditional Chinese medicine grinder, and then sieve them with a 60-mesh stainless steel sieve, and collect the sieved and unsifted materials respectively. For the unscreened broccoli seed powder or rapeseed, return...

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PUM

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Abstract

The invention discloses a new preparation method of 1-isothiocyanic acid-4-methanesulfonyl-(2-ene) butane, and particularly relates to a method for the extraction of sulforaphane from radish seeds or broccoli seeds or rape seeds. According to the method, air-dried radish seeds or broccoli seeds or rape seeds are used as a raw material for preparation of a radish seed crushing liquid, an enzyme deactivated broccoli seed or radish seed dispersion liquid, a degreased fine grinding liquid, a fermentation liquid, a protein removal fermentation liquid, a concentrated liquid, dry polysaccharide powder and high purity sulforaphane freeze-dried powder for preparation of 1-isothiocyanic acid-4-methanesulfonyl-(2-ene) butane with the purity of more than 98%. The production rate of the sulforaphane prepared by the method is high, the operation is simple, and the product has the characteristics of being high in product purity of more than 98%, green, non-pollution and the like. The product prepared by the method can be widely used in medicine and health care industry, and has cancer preventing and resistant function.

Description

1. Technical field [0001] The invention belongs to the technical field of biochemistry, and in particular relates to a method for extracting 1-isothiocyanate-4-methylsulfonyl-(2-ene)butane from radish seeds, broccoli or rape seeds. 2. Background technology [0002] Extensive research in epidemiology and pharmacology has shown that where the incidence of cancer is low, the proportion of vegetables and fruits in people's diet is relatively large, because there are active ingredients in these vegetables and fruits that can prevent or slow down the development of cancer, such as cruciferous Sulforaphane and indoles in vegetables, soybean isoflavones in soybeans, etc. have all been proven to have good anti-cancer and anti-cancer effects. [0003] Modern studies have shown that radish seeds contain a large amount of volatile oils, fats, polysaccharides, proteins, alkaloids, glucosinolates and glucosinosidases. Broccoli, also known as broccoli and broccoli, is a variety of Brassic...

Claims

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Application Information

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IPC IPC(8): C12P13/00A23K1/14A23K1/16A23K20/105
Inventor 刘庆海颜李秀周小华蒋小琴王江杨志雄赵春花
Owner 重庆海巨农业发展有限公司
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