Extracting and purifying method of high-purity sulforaphane

A high-purity technology of sulforaphane, applied in organic chemistry and other fields, can solve problems such as inability to industrialize production, and achieve stable product quality and simple process flow

Inactive Publication Date: 2013-01-30
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for extracting high-purity sulforaphane from broccoli seeds, so as to overcome the defect that the pri

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 100g of broccoli seeds, grind them to 30-60 mesh, add 200ml of water; hydrolyze at 35°C for 8h, add 800ml of absolute ethanol, ultrasonically extract for 30min, the frequency of ultrasonic extraction is 40kHz, and the power is 200W; gauze filter;

[0025] Concentrate the filtrate in vacuum at 40°C to evaporate ethanol; use suction filtration to filter until clear, and use AB-8 macroporous resin column chromatography to remove impurities with 400mL of ethanol with a mass fraction of 30%. , and discard the eluent, then use 600mL of ethanol with a mass fraction of 50% to elute the sulforaphane on the macroporous resin chromatography column, collect the eluate, and then use alumina column chromatography to collect the sulforaphane The eluate was then vacuum-concentrated at 40°C to an oily extract, 5 mg of the concentrated oil was weighed and dissolved in 10 ml of methanol, and then detected by HPLC. The purity of sulforaphane in the product was 60%.

[0026] Dissolve ...

Embodiment 2

[0028] Take 100g of broccoli seeds, grind them to 30-60 mesh, add 200mL of water; hydrolyze at 35℃ for 10h, add 800mL of absolute ethanol, ultrasonically extract for 30min, ultrasonic extraction frequency 40kHz, power 200W; gauze filter;

[0029] The filtrate was vacuum-concentrated and evaporated ethanol at 40°C; it was filtered until clear by suction filtration, and 150 mL of the clear feed liquid was chromatographed on a DM130 macroporous resin column, and impurities were removed with 400 mL of ethanol with a mass fraction of 30%, and Discard the eluate, and then use 600mL of ethanol with a mass fraction of 50% to elute the sulforaphane on the macroporous resin chromatography column, collect the eluate, and then use alumina column chromatography, and collect the sulforaphane eluted liquid, and then vacuum-concentrated at 40°C to an oily extract, weighed 5mg of the concentrated oily substance and dissolved it in 10mL of methanol, and then detected by HPLC, the purity of sulf...

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Abstract

The invention discloses a method for extracting high-purity sulforaphane from broccoli seeds; and the method comprises the following steps of: (1) after crushing dry broccoli seeds, adding water to the dry broccoli seeds to hydrolyze the broccoli seeds, so as to obtain a solid-liquid mixture; (2) adding anhydrous ethanol to the mixture; ultrasonically extracting the mixture; and carrying out suction filtration or double-layer gauze filtering on the mixture; (3) concentrating and evaporating ethanol from a filter liquor in a vacuum state; (4) carrying out chromatography on a material liquor by using a macroporous resin column and eluting the material liquor by using an ethanol solution in a gradient way; (5) collecting an eluting solution containing sulforaphane; carrying out chromatography on the eluting solution by using an alumina column; and concentrating a sulforaphane chromatography solution to form an extract so as to obtain a crude sulforaphane product; (6) adding water to the obtained crude product so as to dissolve the crude product; and extracting the dissolved crude product by using a polar solvent; and (7) collecting an organic layer; and concentrating the organic layer in a vacuum state so as to obtain an oily extract, so that the high-purity sulforaphane is obtained. As the high-purity sulforaphane can be directly extracted from the broccoli seeds and broccoli related materials, the method for extracting the high-purity sulforaphane from the broccoli seeds, disclosed by the invention, has the advantages of simple process, stable product, simple equipment and safety in production and is suitable for enterprises for industrially extracting the sulforaphane.

Description

technical field [0001] The invention relates to a method for extracting and purifying active ingredients in natural products, in particular to a method for extracting high-purity sulforaphane from broccoli seeds. Background technique [0002] According to the statistics of the World Health Organization, the number of deaths due to cancer in the world is as high as 7 million every year. But so far, people have not found a way to conquer cancer. Therefore, studying and controlling tumors is a major topic in the field of life sciences today. Epidemiological and pharmacological studies have shown that where the incidence of cancer is low, the proportion of vegetables and fruits in people's diet is relatively large. The reason is that there are one or more active ingredients in vegetables and fruits that prevent or slow down the development of cancer, such as lycopene in tomatoes, soy isoflavones in soybean products, tannic acid in berries, and cruciferous fruits and vegetables...

Claims

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Application Information

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IPC IPC(8): C07C331/20
Inventor 何珺谢述琼康冀川杨佳年
Owner GUIZHOU UNIV
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