A kind of purification method of Grifeng element

Abstract

The invention belongs to the technical field of medicine and relates to a method for purifying Grifengsu. The method is as follows: the method of supercritical CO2 extraction-macroporous resin adsorption-high-speed countercurrent chromatographic purification is used to obtain Grifengsu, the content of which is as high as 95%, and the content is as high as 95%. Compared with the traditional method, the method of the invention has the advantages of simple technological process, convenient operation, safe production, no pollution, no solvent residue in the product, and is suitable for industrial production.

Description

technical field

[0001] The invention belongs to the technical field of medicines, in particular to a method for extracting and purifying Grifolin from natural plant Grifengol. Background technique

[0002] Griffonin, also known as Lithospermoside, has the molecular formula C 14 h 19 NO 8 , with a molecular weight of 329.31 and a CAS registration number of 63492-69-3, is a cyanogenic glycoside compound in the form of white plume crystals, mp.263-265°C. It mainly exists in various plants such as legumes and ranunculaceae. Among them, the leguminous plant Gryphon unifoliate Griffonia simplicifolia The content of Baill. root is relatively high, and its molecular structure is as follows:

[0003]

[0004] Pharmacological studies have shown that Grifengin has the effect of increasing red blood cell sodium volume, can be used as an anti-sickle cell drug to treat sickle cell disease crisis, and, in Raji cells, has a strong anti-tumor effect on TPA-induced EBV-EA activation ...

Examples

Embodiment 1

[0016] Take the single-leaf Grifeng root, crush it to 20 mesh, take 1kg and put it into the extraction kettle, set the equipment parameters as follows: extraction temperature 50°C, extraction pressure 30MPa, desorption kettle Ⅰ temperature 33℃, pressure 19MPa, desorption kettle Ⅱ temperature The temperature is 27°C, the pressure is 5MPa, and the supercritical CO 2 , to regulate CO 2 The flow rate was 18 L / h, entraining 440 ml of 70% propylene glycol, extracting for 60 min, analyzing and recovering the reagent, and obtaining the extract. Dissolve and disperse the extract in water, pass it through an AB-8 macroporous adsorption resin column, elute with water until colorless, then elute with 60% ethanol, collect the eluate, concentrate under reduced pressure to obtain the extract. Mix chloroform, methanol, and water in a volume ratio of 6:4:4, take the upper phase as the stationary phase, and the lower phase as the mobile phase, turn on the host of the high-speed countercurrent ...

Embodiment 2

[0018] Take the single-leaf Gelifeng root, crush it to 20 mesh, take 1kg and put it into the extraction kettle, set the equipment parameters as follows: extraction temperature 55°C, extraction pressure 25MPa, analysis kettle Ⅰ temperature 35℃, pressure 23MPa, analysis kettle Ⅱ temperature 25°C, pressure 4MPa, supercritical CO 2 , to regulate CO 2 The flow rate was 18L / h, 520ml of 70% propylene glycol was entrained, extracted for 120min, and the reagent was analyzed and recovered to obtain the extract. The extract was dissolved and dispersed in water, passed through a DM310 macroporous adsorption resin column, first eluted with water until it was colorless, and then eluted with 55% ethanol, the eluate was collected, concentrated under reduced pressure to obtain the extract. Mix chloroform, methanol, and water in a volume ratio of 5:3:3, take the upper phase as the stationary phase, and the lower phase as the mobile phase, turn on the host of the high-speed countercurrent chrom...

Embodiment 3

[0020] Take the single-leaf Grifeng root, crush it to 20 mesh, take 1kg and put it into the extraction kettle, set the equipment parameters as follows: extraction temperature 45°C, extraction pressure 32MPa, analysis kettle Ⅰ temperature 38℃, pressure 21MPa, analysis kettle Ⅱ temperature 30°C, pressure 6MPa, supercritical CO 2 , to regulate CO 2 The flow rate was 18 L / h, entraining 600 ml of 70% propylene glycol, extracting for 30 min, analyzing and recovering the reagent, and obtaining the extract. Dissolve and disperse the extract in water, pass it through a HZ830 macroporous adsorption resin column, elute with water until it becomes colorless, then elute with 50% ethanol, collect the eluate, and concentrate under reduced pressure to obtain the extract. Mix chloroform, methanol, and water in a volume ratio of 4:3:3, take the upper phase as the stationary phase, and the lower phase as the mobile phase, turn on the host of the high-speed countercurrent chromatograph, adjust t...

technical field

[0001] The invention belongs to the technical field of medicines, in particular to a method for extracting and purifying Grifolin from natural plant Grifengol. Background technique

[0002] Griffonin, also known as Lithospermoside, has the molecular formula C 14 h 19 NO 8 , with a molecular weight of 329.31 and a CAS registration number of 63492-69-3, is a cyanogenic glycoside compound in the form of white plume crystals, mp.263-265°C. It mainly exists in various plants such as legumes and ranunculaceae. Among them, the leguminous plant Gryphon unifoliate Griffonia simplicifolia The content of Baill. root is relatively high, and its molecular structure is as follows:

[0003]

[0004] Pharmacological studies have shown that Grifengin has the effect of increasing red blood cell sodium volume, can be used as an anti-sickle cell drug to treat sickle cell disease crisis, and, in Raji cells, has a strong anti-tumor effect on TPA-induced EBV-EA activation ...

Examples

Embodiment 1

[0016] Take the single-leaf Grifeng root, crush it to 20 mesh, take 1kg and put it into the extraction kettle, set the equipment parameters as follows: extraction temperature 50°C, extraction pressure 30MPa, desorption kettle Ⅰ temperature 33℃, pressure 19MPa, desorption kettle Ⅱ temperature The temperature is 27°C, the pressure is 5MPa, and the supercritical CO 2 , to regulate CO 2 The flow rate was 18 L / h, entraining 440 ml of 70% propylene glycol, extracting for 60 min, analyzing and recovering the reagent, and obtaining the extract. Dissolve and disperse the extract in water, pass it through an AB-8 macroporous adsorption resin column, elute with water until colorless, then elute with 60% ethanol, collect the eluate, concentrate under reduced pressure to obtain the extract. Mix chloroform, methanol, and water in a volume ratio of 6:4:4, take the upper phase as the stationary phase, and the lower phase as the mobile phase, turn on the host of the high-speed countercurrent ...

Embodiment 2

[0018] Take the single-leaf Gelifeng root, crush it to 20 mesh, take 1kg and put it into the extraction kettle, set the equipment parameters as follows: extraction temperature 55°C, extraction pressure 25MPa, analysis kettle Ⅰ temperature 35℃, pressure 23MPa, analysis kettle Ⅱ temperature 25°C, pressure 4MPa, supercritical CO 2 , to regulate CO 2 The flow rate was 18L / h, 520ml of 70% propylene glycol was entrained, extracted for 120min, and the reagent was analyzed and recovered to obtain the extract. The extract was dissolved and dispersed in water, passed through a DM310 macroporous adsorption resin column, first eluted with water until it was colorless, and then eluted with 55% ethanol, the eluate was collected, concentrated under reduced pressure to obtain the extract. Mix chloroform, methanol, and water in a volume ratio of 5:3:3, take the upper phase as the stationary phase, and the lower phase as the mobile phase, turn on the host of the high-speed countercurrent chrom...

Embodiment 3

[0020] Take the single-leaf Grifeng root, crush it to 20 mesh, take 1kg and put it into the extraction kettle, set the equipment parameters as follows: extraction temperature 45°C, extraction pressure 32MPa, analysis kettle Ⅰ temperature 38℃, pressure 21MPa, analysis kettle Ⅱ temperature 30°C, pressure 6MPa, supercritical CO 2 , to regulate CO 2 The flow rate was 18 L / h, entraining 600 ml of 70% propylene glycol, extracting for 30 min, analyzing and recovering the reagent, and obtaining the extract. Dissolve and disperse the extract in water, pass it through a HZ830 macroporous adsorption resin column, elute with water until it becomes colorless, then elute with 50% ethanol, collect the eluate, and concentrate under reduced pressure to obtain the extract. Mix chloroform, methanol, and water in a volume ratio of 4:3:3, take the upper phase as the stationary phase, and the lower phase as the mobile phase, turn on the host of the high-speed countercurrent chromatograph, adjust t...

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