Method for extracting and separating various components from flaxseed meal based on subcritical composite solvent

Patent metadata

Field	Value
Publication number	US-12465874-B2
Application number	US-202218011529-A
Country	US
Kind code	B2
Filing date	Jul 18, 2022
Priority date	Aug 4, 2021
Publication date	Nov 11, 2025
Grant date	Nov 11, 2025

Abstract

Disclosed in the present disclosure is a method for extracting and separating various components from flaxseed meal based on a subcritical composite solvent, including the following steps: adding an extraction agent to flaxseed meal for subcritical extraction to obtain a crude flax lignan extract and crude flaxseed oil in one step, where the extraction agent includes n-butane and anhydrous ethanol at a volume ratio of 1:1; adding n-hexane to the crude flaxseed oil for fractional extraction, and conducting rotary evaporation to obtain flaxseed oil; and subjecting the flaxseed meal used to hot water extraction to obtain flaxseed gum. In the present disclosure, the subcritical composite solvent used in an extraction process can replace a large number of organic reagents used in a traditional extraction process, and has the characteristics of good solvent effect, environmental friendliness, recyclability, and low burden on the environment.

First claim

What is claimed is:

1 . A method for extracting and separating various components from flaxseed meal based on a subcritical composite solvent, comprising the following steps:
(1) adding an extraction agent to flaxseed meal for subcritical extraction, and after the extraction is completed, obtaining a crude lignan extract in an upper extract and crude flaxseed oil in a lower extract, wherein the extraction agent comprises n-butane and anhydrous ethanol at a volume ratio of 1:1; (2) adding n-hexane to the crude flaxseed oil obtained in step (1) for fractional extraction to obtain a supernatant, and subjecting the supernatant to concentration by rotary evaporation until the volume is unchanged to obtain flaxseed oil; and (3) subjecting the flaxseed meal used after step (1) to hot water extraction to obtain flaxseed gum.

2 . The extraction and separation method according to claim 1 , wherein in step (1), the subcritical extraction is conducted at 69° C. for 2 hours.

3 . The extraction and separation method according to claim 1 , wherein the obtained crude lignan extract is subjected to rotary evaporation to remove the residual extraction agent, and then subjected to centrifugation to obtain a supernatant containing a lignan polymer; and the supernatant is subjected to alkali treatment, acid neutralization, chromatography with macroporous adsorption resin, and column chromatography with silica gel to obtain a lignan.

4 . The extraction and separation method according to claim 3 , wherein the column chromatography with silica gel comprises conducting elution with dichloromethane, a mixture of dichloromethane, methanol, and glacial acetic acid at a ratio of 10:1:0.1 (V/V/V), a mixture of dichloromethane, methanol, and glacial acetic acid at a ratio of 10:2:0.1 (V/V/V), and a mixture of dichloromethane, methanol, and glacial acetic acid at a ratio of 10:2.5:0.1 (V/V/V) in sequence, and collecting all tube solutions comprising a secoisolariciresinol diglucoside (SDG) component.

5 . The extraction and separation method according to claim 3 , wherein the alkali treatment comprises adding a 0.1 M sodium hydroxide solution for alkali hydrolysis at room temperature for at least 24 hours.

6 . The extraction and separation method according to claim 3 , wherein the acid neutralization comprises adding acetic acid until the pH value of the system is 7.

7 . The extraction and separation method according to claim 3 , wherein the chromatography with macroporous adsorption resin comprises adsorption with AB-8 macroporous resin.

8 . The extraction and separation method according to claim 7 , wherein the chromatography with macroporous adsorption resin comprises elution with an ethanol solution with a V/V percentage of 70% to obtain an eluent containing a lignan.

9 . The extraction and separation method according to claim 1 , wherein in step (2), the fractional extraction is conducted at 70° C. for 3-5 hours.

10 . The extraction and separation method according to claim 1 , wherein in step (3), the hot water extraction comprises water extraction at 70° C., 400 rpm, and a material-liquid ratio of 1:25 for 2 hours.

Assignees

• Univ Jinan

Inventors

• Li Ying
• Zhang Ning
• Wang Yong

Classifications

• C11B3/006

  by extraction · CPC title

• C11B1/10

  by extracting · CPC title

• C08B37/006

  Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof · CPC title

• C07H15/203 Primary

  Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems · CPC title

• C07H1/06

  Separation; Purification · CPC title