Method for extracting high-purity vasicine from adhatoda vasica

Abstract

The invention aims at providing a method capable of extracting high-purity vasicine from adhatoda vasica. The high-purity vasicine is prepared by the following methods: after microbial fermentation is performed, performing extracting by using an ethanol solution, filtering, degreasing, vacuum concentration, affinity chromatography, ion-exchange column chromatography, crystallization and the like. A product of the invention has the effects of remarkable uterus excitation effect and the ability of reducing myocardial contractility, reducing coronary artery flow and slightly lowering blood pressure, and also has a good expansion effect on bronchi.

Description

technical field

[0001] The invention belongs to the field of natural product processing, and relates to a method for extracting high-purity orchidine from duckbill flowers. Background technique

[0002] Duck-billed flower is also called big resurgence, big rebuff bone, big joint bone, etc. It is an evergreen shrub of the family Acanthaceae Duck-billed flower. It is mainly distributed in southeastern Asia, in Guangdong, Guangxi, Hainan, Macau, Hong Kong, Yunnan and other places in my country. Productive, or cultivated, or wild. The main characteristics of the plant are: large shrub, up to 1-3 meters; branches cylindrical, gray, with lenticels, young branches densely covered with off-white puberulent. Leaves papery, oblong-lanceolate to lanceolate, or ovate or elliptic-ovate, 15-20 cm long, 4.5-7.5 cm wide, apex acuminate, sometimes slightly caudate, base broadly cuneate, Margin entire, subglabrous above, puberulent abaxially; midvein grooved above, lateral veins about 12 on ...

Examples

Embodiment 1

[0026] Crush the dried duckbill flower stem and leaf raw materials to 10-20 mesh, weigh 100Kg, add 10L of Aspergillus crassasporium culture solution, and carry out aerobic solid fermentation at 28-30°C for 3-5 days. After fermentation, add 800L of 60-80% ethanol to Duckbill flower, ultrasonically extract 3 times at room temperature, 30 minutes each time, filter twice with three layers of gauze, filter once with ceramic membrane, combine the filtrates, and concentrate under reduced pressure at 50°C to obtain dry matter 6.2kg; extract the dry matter with 45L of petroleum ether, filter it once with a ceramic membrane, and concentrate the filtrate under reduced pressure at 50°C to recover petroleum ether; obtain a filter residue of 3.72kg, add 3L of alkaline water with pH=9 to dissolve, and dissolve it with a ceramic membrane Filter once, carry out adsorption separation on the macroporous adsorption resin D101 on the filtrate, and concentrate and dry the 30% ethanol phase eluate co...

Embodiment 2

[0030]Crush the dried duckbill flower stem and leaf raw materials to 10-20 mesh, weigh 200Kg, add 15L Aspergillus crassasporium culture solution, and carry out aerobic solid fermentation at 28-30°C for 3-5 days. After fermentation, Duckbill flower was extracted with 1800L of 60-80% ethanol, ultrasonically extracted 3 times at room temperature, 30min each time, filtered twice with three layers of gauze, once with ceramic membrane, combined filtrates, concentrated under reduced pressure at 50°C to obtain dry matter 11.4 kg; extract the dry matter with 90L of petroleum ether, filter it once with a ceramic membrane, concentrate the filtrate under reduced pressure at 50°C to recover petroleum ether; obtain 7.4kg of filter residue, add 7L of alkaline water with pH=9 to dissolve, and filter with a ceramic membrane Once, the macroporous adsorption resin D101 on the filtrate was adsorbed and separated, and the collected 30% ethanol phase eluate was concentrated and dried under reduced p...

Embodiment 3

[0032] Crush the dried duckbill flower stem and leaf raw material to 10-20 mesh, weigh 5Kg, add 0.5L Aspergillus crassasporium culture solution, and carry out aerobic solid fermentation at 28-30°C for 3-5 days. After fermentation, Duckbill flower was extracted with 40L of 60-80% ethanol, ultrasonically extracted 3 times at room temperature, 30 minutes each time, filtered twice with three layers of gauze, once with ceramic membrane, combined filtrates, concentrated under reduced pressure at 50°C to obtain 295g of dry matter ;Leach the dry matter with 2.5L of petroleum ether, filter it once with a ceramic membrane, concentrate the filtrate under reduced pressure at 50°C to recover petroleum ether; obtain 187g of filter residue, add 0.2L of alkaline water with pH=9 to dissolve, and filter with a ceramic membrane Once, the macroporous adsorption resin D101 on the filtrate is adsorbed and separated, and the collected 30% ethanol phase eluate is concentrated and dried under reduced p...

technical field

[0001] The invention belongs to the field of natural product processing, and relates to a method for extracting high-purity orchidine from duckbill flowers. Background technique

[0002] Duck-billed flower is also called big resurgence, big rebuff bone, big joint bone, etc. It is an evergreen shrub of the family Acanthaceae Duck-billed flower. It is mainly distributed in southeastern Asia, in Guangdong, Guangxi, Hainan, Macau, Hong Kong, Yunnan and other places in my country. Productive, or cultivated, or wild. The main characteristics of the plant are: large shrub, up to 1-3 meters; branches cylindrical, gray, with lenticels, young branches densely covered with off-white puberulent. Leaves papery, oblong-lanceolate to lanceolate, or ovate or elliptic-ovate, 15-20 cm long, 4.5-7.5 cm wide, apex acuminate, sometimes slightly caudate, base broadly cuneate, Margin entire, subglabrous above, puberulent abaxially; midvein grooved above, lateral veins about 12 on ...

Examples

Embodiment 1

[0026] Crush the dried duckbill flower stem and leaf raw materials to 10-20 mesh, weigh 100Kg, add 10L of Aspergillus crassasporium culture solution, and carry out aerobic solid fermentation at 28-30°C for 3-5 days. After fermentation, add 800L of 60-80% ethanol to Duckbill flower, ultrasonically extract 3 times at room temperature, 30 minutes each time, filter twice with three layers of gauze, filter once with ceramic membrane, combine the filtrates, and concentrate under reduced pressure at 50°C to obtain dry matter 6.2kg; extract the dry matter with 45L of petroleum ether, filter it once with a ceramic membrane, and concentrate the filtrate under reduced pressure at 50°C to recover petroleum ether; obtain a filter residue of 3.72kg, add 3L of alkaline water with pH=9 to dissolve, and dissolve it with a ceramic membrane Filter once, carry out adsorption separation on the macroporous adsorption resin D101 on the filtrate, and concentrate and dry the 30% ethanol phase eluate co...

Embodiment 2

[0030]Crush the dried duckbill flower stem and leaf raw materials to 10-20 mesh, weigh 200Kg, add 15L Aspergillus crassasporium culture solution, and carry out aerobic solid fermentation at 28-30°C for 3-5 days. After fermentation, Duckbill flower was extracted with 1800L of 60-80% ethanol, ultrasonically extracted 3 times at room temperature, 30min each time, filtered twice with three layers of gauze, once with ceramic membrane, combined filtrates, concentrated under reduced pressure at 50°C to obtain dry matter 11.4 kg; extract the dry matter with 90L of petroleum ether, filter it once with a ceramic membrane, concentrate the filtrate under reduced pressure at 50°C to recover petroleum ether; obtain 7.4kg of filter residue, add 7L of alkaline water with pH=9 to dissolve, and filter with a ceramic membrane Once, the macroporous adsorption resin D101 on the filtrate was adsorbed and separated, and the collected 30% ethanol phase eluate was concentrated and dried under reduced p...

Embodiment 3

[0032] Crush the dried duckbill flower stem and leaf raw material to 10-20 mesh, weigh 5Kg, add 0.5L Aspergillus crassasporium culture solution, and carry out aerobic solid fermentation at 28-30°C for 3-5 days. After fermentation, Duckbill flower was extracted with 40L of 60-80% ethanol, ultrasonically extracted 3 times at room temperature, 30 minutes each time, filtered twice with three layers of gauze, once with ceramic membrane, combined filtrates, concentrated under reduced pressure at 50°C to obtain 295g of dry matter ;Leach the dry matter with 2.5L of petroleum ether, filter it once with a ceramic membrane, concentrate the filtrate under reduced pressure at 50°C to recover petroleum ether; obtain 187g of filter residue, add 0.2L of alkaline water with pH=9 to dissolve, and filter with a ceramic membrane Once, the macroporous adsorption resin D101 on the filtrate is adsorbed and separated, and the collected 30% ethanol phase eluate is concentrated and dried under reduced p...