Method for separating 4-methylsulphinyl-3-cyclobutenyl glucosinolates

A technology of methylsulfinyl and butenyl sulfide, applied in the field of food processing, can solve the problems of less separation, high cost of glucosinolates, large separation technology, etc.

Inactive Publication Date: 2008-01-09
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The existing separation of glucosinolates mainly uses preparative high-performance liquid chromatography, and its limitation is that the amount of separation is small
Secondly, high-performance liquid chromatograp...

Method used

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  • Method for separating 4-methylsulphinyl-3-cyclobutenyl glucosinolates
  • Method for separating 4-methylsulphinyl-3-cyclobutenyl glucosinolates
  • Method for separating 4-methylsulphinyl-3-cyclobutenyl glucosinolates

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Effect test

Embodiment 1

[0022] The solvent system of the present embodiment adopts n-butanol-acetonitrile-5% ammonium sulfate solution (10:5:4); The countercurrent chromatograph is HSCCC-D1000 high-speed countercurrent chromatograph (column capacity 1L), and GRE in the crude extract of GRE is about 15%.

[0023] Measure 2000ml of n-butanol, 1000ml of acetonitrile, and 800ml of 5% ammonium sulfate solution, put it in a 5L separatory funnel, shake it well, and put the upper and lower phases into reagent bottles after standing for stratification. The lower phase was injected into the chromatographic column of high-speed countercurrent chromatography at a flow rate of 10 ml / min. Weigh 2.0 g of the GRE crude extract and dissolve it in 50 ml upper phase to prepare a countercurrent chromatography sample solution, turn on the countercurrent chromatograph to 800 rpm, and then input the sample solution at a flow rate of 1.0ml / min. The flow rate of 2.0ml / min was input into the mobile phase to elute the compone...

Embodiment 2

[0025] The solvent system of the present embodiment adopts n-butanol-acetonitrile-5% ammonium sulfate solution (10:3:4); About 15%.

[0026] Measure 8L of n-butanol, 2.7L of acetonitrile, and 3.2L of 5% ammonium sulfate solution, put them in a 20L separatory bottle, mix thoroughly, and after standing for stratification, put the upper and lower phases into the reagent bottle respectively. Inject the lower phase into the chromatographic column of the low-speed countercurrent chromatography at a flow rate of 20ml / min until the chromatographic column is completely filled. Weigh 30.0g of the GRE crude extract and dissolve it in 500ml upper phase to prepare a countercurrent chromatography sample solution, turn on the countercurrent chromatograph to 50 rpm, and then input the sample solution at a flow rate of 2.0ml / min. The flow rate of 5.0ml / min was input into the mobile phase to elute the components in the column, and the countercurrent chromatographic effluent was detected at 235...

Embodiment 3

[0028] The solvent system of the present embodiment adopts n-butanol-acetonitrile-5% ammonium sulfate solution (10:6:4); The countercurrent chromatograph is RSCCC-D40000 low-speed countercurrent chromatograph (column capacity 40L), and GRE in the crude extract of GRE is about 15%.

[0029] Measure 80L of n-butanol, 48L of acetonitrile, and 32L of 5% ammonium sulfate solution, place them in a 200L separatory tank, mix thoroughly, and after standing for stratification, put the upper and lower phases into reagent bottles respectively. The lower phase is injected into the chromatographic column of the low-speed countercurrent chromatography at a flow rate of 200ml / min until the chromatographic column is completely filled. Weigh 300.0g of the GRE crude extract and dissolve it in 5000ml upper phase to prepare a countercurrent chromatography sample solution, turn on the countercurrent chromatograph to 50 rpm, and then input the sample solution at a flow rate of 10.0ml / min. The flow ...

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Abstract

A method for preparing GRE by separating from radish seed is carried out by leaching thio-glucoside by boiling methanol, separating and purifying GRE from radish seed coarse extract with countercurrent chromatography as separator. The solvent system consists of n-butyl alcohol, methyl cyanide and 10% ammonia sulfate solution in proportion of 10:3-6:5. It's economical and cheap and has purity above 87%.

Description

technical field [0001] The invention belongs to the technical field of food processing, and relates to a deep processing technology of radish seeds, in particular to a method for separating and preparing 4-methylsulfinyl-3-butenyl glucosinolate (GRE) from radish seeds. technical background [0002] Radish is a traditional edible vegetable in my country. It has high nutritional and health value, and is rich in nutrients and active substances. Glucosinolates are the main active ingredients. The main component of glucosinolate in radish seeds is 4-methylsulfinyl-3-butenyl glucosinolate (GRE). Studies at home and abroad have shown that the degradation products of GRE have biological activities such as anti-allergic, anti-cancer, and antibacterial. [0003] The existing separation of glucosinolates mainly uses preparative high-performance liquid chromatography, and its limitation is that the amount of separation is small. Secondly, high-performance liquid chromatography columns...

Claims

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Application Information

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IPC IPC(8): C07H15/14C07H1/08
Inventor 杜琪珍王科沈莲清
Owner ZHEJIANG GONGSHANG UNIVERSITY
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