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Method for preparing secoisolariciresinol diglucoside

A technology of flax lignans and ethanol aqueous solution, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of complicated process and long production cycle, and achieve simplified process, reduced hydrolysis time, shortened The effect of the production cycle

Inactive Publication Date: 2011-05-11
GUILIN NATURAL INGREDIENTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the water precipitation step in this method still needs 12 to 24 hours, the production cycle of this method is still relatively long. In addition, this method also needs a second deesterification process, and the process is relatively complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation method of embodiment 1 flax lignans comprises the following steps:

[0019] 1) Take linseed and crush it, extract it with 80% (v / v) ethanol aqueous solution equivalent to 10 times the weight of the raw material in a water bath at 80°C for 2 hours, filter, and concentrate the obtained extract to 2 times the weight of the raw material to obtain concentrated liquid;

[0020] 2) Add aqueous sodium hydroxide solution (30%, w / w) to the concentrated solution until the concentration of sodium hydroxide in the concentrated solution is 3% (mass), hydrolyze at 50°C for 30min, cool, add acid to adjust pH=3.5 , place for 30min, centrifuge, and collect the supernatant;

[0021] 3) The supernatant enters the DM133 type macroporous resin column for adsorption, washes the resin column with water equivalent to 20 times the weight of the raw material, and then elutes with 50% (v / v) ethanol aqueous solution equivalent to 5 times the weight of the raw material, and collects...

Embodiment 2

[0023] The preparation method of embodiment 2 flax lignans comprises the following steps:

[0024] 1) Take linseed and pulverize it, extract it with an aqueous ethanol solution equivalent to 8 times the weight of the raw material and 50% (v / v) in a water bath at 70°C for 2 hours, filter, and then use the filter residue equivalent to 7 times the weight of the raw material and 50% ( v / v) was extracted in an ethanol aqueous solution at 80° C. for 1.5 hours, filtered, and the extracts were combined, and the obtained extract was concentrated to twice the weight of the raw material to obtain a concentrated solution;

[0025] 2) Add aqueous sodium hydroxide solution (40%, w / w) to the concentrated solution until the concentration of sodium hydroxide in the concentrated solution is 4% (mass), hydrolyze at 60°C for 40min, cool, and add acid to adjust pH=4 , place for 30min, centrifuge, and collect the supernatant;

[0026] 3) The supernatant enters the DM2 type macroporous resin column...

Embodiment 3

[0028] The preparation method of embodiment 3 flax lignans comprises the following steps:

[0029] 1) Take linseed and pulverize it, extract it with 70% (v / v) ethanol aqueous solution equivalent to 9 times the weight of the raw material for 3 hours at 75°C in a water bath, filter, and then use 80% (v / v) equivalent to 10 times the weight of the raw material to filter the residue v / v) ethanol aqueous solution was extracted for 1 hour at 70°C in a water bath, filtered, the extracts were combined, and the obtained extract was concentrated to 2.5 times the weight of the raw material to obtain a concentrated solution;

[0030] 2) Add potassium hydroxide aqueous solution (30%, w / w) to the concentrate until the concentration of potassium hydroxide in the concentrate is 2% (mass), hydrolyze at 80°C for 30min, cool, add acid to adjust pH=4.5 , place for 35min, centrifuge, and collect the supernatant;

[0031] 3) The supernatant enters the HP-20 type macroporous resin column for adsorpt...

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Abstract

The invention discloses a method for preparing secoisolariciresinol diglucoside (SDG), which comprises the following steps of: 1) crushing linseeds, extracting by using ethanol aqueous solution, and concentrating extracting solution to obtain concentrated solution; 2) adding alkaline aqueous solution into the concentrated solution, hydrolyzing at the temperature of between 50 and 80 DEG C for 30 to 40 minutes, cooling, regulating the pH to 3.5 to 4.5 by adding acid, standing for 30 to 40 minutes, centrifuging and collecting supernatant; and 3) adsorbing the supernatant through a macroporous resin column, washing the resin column until effluent liquid is not saline, eluting by using 25 to 50 volume percent ethanol aqueous solution, collecting the eluent, concentrating under reduced pressure and drying to prepare the SDG. The method is simple in process and is easily controlled, the extraction time and the hydrolysis time are greatly reduced, the production cycle is effectively shortened, the quality requirement of a product obtained by the method is met, the SDG content in the product is 30 to 50 percent, and the product yield is 3 to 5 percent.

Description

technical field [0001] The invention relates to a preparation method of flax lignans. Background technique [0002] Flax lignans are a class of lignans that come from flaxseed. Currently at least 8 components have been isolated from flaxseed, among which the one with the most content and beneficial to the human body is called "secoisolarix resinol diglucoside", or SDG for short. Flax lignans have attracted great attention in dietary and healthcare applications due to their broad-spectrum biological activities such as antitumor, antiviral, and antioxidative. [0003] As early as the 1950s, it was reported that flaxseeds were extracted with ethanol and dioxane solvents, and then hydrolyzed by sodium methoxide or barium methoxide in anhydrous methanol to prepare flax lignans. Improve to extract with ethanol aqueous solution later, the method for sodium hydroxide hydrolysis and resin chromatography purification, as the Chinese invention patent of publication number CN1394865, ...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/08
Inventor 宋云飞梁远盛赵军孙步祥汤凌志
Owner GUILIN NATURAL INGREDIENTS CORP
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