Method for extracting antofine

Abstract

The invention discloses a method for extracting antofine. The method comprises the following steps of: crushing a cynanchum komarovii raw material, adding 0.5 to 1 percent aqueous solution of hydrochloric acid or sulfuric acid, extracting, regulating the pH of the extract to be between 7.5 and 8.5, adding an ultra-filtration membrane for ultra-filtration, adding a nano-filtration membrane for nano-filtration, regulating the pH of the concentrate to be between 9.5 and 11, extracting the concentrate by using chloroform, separating the concentrated extract by adopting preparative liquid chromatography, performing ultraviolet on-line detection, collecting the target component, drying the target component at a low temperature, and thus obtaining the antofine product. The method is low in energy consumption, low in pollution and high in product content (which can reach over 95 percent), is suitable for small experiments, and can also be used for industrialized production.

Description

technical field

[0001] The invention belongs to the technical field of extraction and separation of traditional Chinese medicines, and in particular relates to an extraction method of anthofen. Background technique

[0002] Laoguatou is a plant of the genus Goosedown Vine in the family Romoaceae, also known as Niuxinpu. It is used in folk medicine. The whole plant is used as medicine, which has the effects of promoting blood circulation, relieving pain, and reducing inflammation.

[0003] Antorfen is the main active ingredient of Laoguatou, which is an isoquinoline alkaloid, light yellow needle crystal (dichloromethane-methanol), molecular formula C 23 h 25 NO 3 , the structural formula:

[0004]

[0005] Antorfen has strong cytotoxic activity on K-562, HL-60 and Hela cells, and the inhibition rate on P388 is 73.1% when the concentration is 1mg / ml. Antorfen has antibacterial effect, and has significant inhibitory effect on Bacillus subtilis, Micrococcus luteus and Esc...

Examples

Embodiment 1

[0021] Grind the old melon head raw material, take 1kg, add 1% hydrochloric acid aqueous solution to soak for 3 hours, ultrasonically treat for 40 minutes, filter to obtain the extract, adjust the pH to 7.5, add ultrafiltration with a molecular weight cut-off of 3000, and then add a molecular weight cut-off of 200 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 10, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; Membrane filtration to obtain the sample solution, the extraction column is filled with C8 bonded phase, the particle size is 10 μm, the column length is 15 cm, and the diameter is 4 cm. Diamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 50ml / min, and the ultraviolet on-line detection was performed at a detection wavelength of 258nm. The target components were collected and dried at low temperature to ...

Embodiment 2

[0023] Grind the old melon head raw material, take 1kg, add 0.5% sulfuric acid aqueous solution to soak for 8 hours, ultrasonically treat for 45 minutes, filter to obtain the extract, adjust the pH to 8.5, add ultrafiltration with a molecular weight cut-off of 5000, and then add a molecular weight cut-off of 500 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 9.5, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; the crude product is dissolved in 95% ethanol to form a solution with a concentration of 100mg / ml, and the solution is subjected to 0.45 μm microfiltration membrane to obtain the sample solution, the extraction column is filled with C18 bonded phase, the particle size is 20 μm, the column length is 10 cm, and the diameter is 1 cm. The % ethylenediamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 10ml / min...

Embodiment 3

[0025] Grind the old melon head raw material, take 5kg, add 0.8% sulfuric acid aqueous solution to soak for 6 hours, ultrasonically treat for 35 minutes, filter to obtain the extract, adjust the pH to 8, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 5000, and then add a molecular weight cut-off of 300 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 11, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; Membrane filtration to obtain the sample solution, the extraction column is filled with C18 bonded phase, the particle size is 15 μm, the column length is 50 cm, and the diameter is 10 cm. Diamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 250ml / min, and the ultraviolet on-line detection was performed at a detection wavelength of 258nm. The target components were collected and drie...

technical field

[0001] The invention belongs to the technical field of extraction and separation of traditional Chinese medicines, and in particular relates to an extraction method of anthofen. Background technique

[0002] Laoguatou is a plant of the genus Goosedown Vine in the family Romoaceae, also known as Niuxinpu. It is used in folk medicine. The whole plant is used as medicine, which has the effects of promoting blood circulation, relieving pain, and reducing inflammation.

[0003] Antorfen is the main active ingredient of Laoguatou, which is an isoquinoline alkaloid, light yellow needle crystal (dichloromethane-methanol), molecular formula C 23 h 25 NO 3 , the structural formula:

[0004]

[0005] Antorfen has strong cytotoxic activity on K-562, HL-60 and Hela cells, and the inhibition rate on P388 is 73.1% when the concentration is 1mg / ml. Antorfen has antibacterial effect, and has significant inhibitory effect on Bacillus subtilis, Micrococcus luteus and Esc...

Examples

Embodiment 1

[0021] Grind the old melon head raw material, take 1kg, add 1% hydrochloric acid aqueous solution to soak for 3 hours, ultrasonically treat for 40 minutes, filter to obtain the extract, adjust the pH to 7.5, add ultrafiltration with a molecular weight cut-off of 3000, and then add a molecular weight cut-off of 200 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 10, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; Membrane filtration to obtain the sample solution, the extraction column is filled with C8 bonded phase, the particle size is 10 μm, the column length is 15 cm, and the diameter is 4 cm. Diamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 50ml / min, and the ultraviolet on-line detection was performed at a detection wavelength of 258nm. The target components were collected and dried at low temperature to ...

Embodiment 2

[0023] Grind the old melon head raw material, take 1kg, add 0.5% sulfuric acid aqueous solution to soak for 8 hours, ultrasonically treat for 45 minutes, filter to obtain the extract, adjust the pH to 8.5, add ultrafiltration with a molecular weight cut-off of 5000, and then add a molecular weight cut-off of 500 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 9.5, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; the crude product is dissolved in 95% ethanol to form a solution with a concentration of 100mg / ml, and the solution is subjected to 0.45 μm microfiltration membrane to obtain the sample solution, the extraction column is filled with C18 bonded phase, the particle size is 20 μm, the column length is 10 cm, and the diameter is 1 cm. The % ethylenediamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 10ml / min...

Embodiment 3

[0025] Grind the old melon head raw material, take 5kg, add 0.8% sulfuric acid aqueous solution to soak for 6 hours, ultrasonically treat for 35 minutes, filter to obtain the extract, adjust the pH to 8, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 5000, and then add a molecular weight cut-off of 300 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 11, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; Membrane filtration to obtain the sample solution, the extraction column is filled with C18 bonded phase, the particle size is 15 μm, the column length is 50 cm, and the diameter is 10 cm. Diamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 250ml / min, and the ultraviolet on-line detection was performed at a detection wavelength of 258nm. The target components were collected and drie...

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