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Method for extracting 4-hydroxyderricin from angelica keiskei

A hydroxyl and extract technology, applied in the biological field, can solve the problems of small preparation amount, high cost, and long cycle, and achieve the effect of large amount of preparation, short preparation cycle, and low solution efficiency

Inactive Publication Date: 2013-02-06
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing preparation process has the disadvantages of low yield, high cost, small preparation amount and long cycle

Method used

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  • Method for extracting 4-hydroxyderricin from angelica keiskei

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Ashitaba was crushed, 500g was taken and 5 times the amount of 60% ethanol was ultrasonically extracted for 3 times, the extract was concentrated to no alcohol, added to a polyamide resin column for adsorption, 4BV30% ethanol solution was taken for elution, the eluate was collected and concentrated, adjusted to ph3, added An equal volume of ethyl acetate was extracted three times, the extract was washed three times with 5% sodium carbonate solution, and the ethyl acetate was recovered to obtain 8 g of crude product. Mix n-hexane, ethyl acetate, methanol, and water in a ratio of 3:3:2:3, and after standing for stratification, take the upper phase and fill the high-speed countercurrent chromatography column, turn the host, adjust the speed to 800rpm, and pump into the lower phase for flow Phase, after the dynamic equilibrium is established, the flow rate is adjusted to 2ml / min, and the crude product dissolved in the mobile phase is injected by the injection valve, and the ...

Embodiment 2

[0018] Ashitaba was crushed, and 500g was taken and 8 times the amount of 30% ethanol was ultrasonically extracted twice, the extract was concentrated to no alcohol, added to a polyamide resin column for adsorption, 5BV20% ethanol solution was taken for elution, the eluate was collected and concentrated, adjusted to ph5, added Equal volume of ethyl acetate was extracted 3 times, the extract was washed 4 times with 5% sodium carbonate solution, and the ethyl acetate was recovered to obtain 7 g of crude product. Mix n-hexane, ethyl acetate, methanol, and water in a ratio of 7:7:4:3, and after standing for stratification, take the upper phase and fill the high-speed countercurrent chromatography column, turn the host, adjust the speed to 900rpm, and pump into the lower phase for flow Phase, after the dynamic equilibrium is established, the flow rate is adjusted to 3ml / min. At the same time, the crude product dissolved in the mobile phase is injected by the injection valve, monitor...

Embodiment 3

[0020] Ashitaba is crushed, and 500g is taken and 8 times the amount of 40% ethanol is ultrasonically extracted twice, the extract is concentrated to no alcohol, added to a polyamide resin column for adsorption, eluted with 5BV30% ethanol solution, and the eluate is collected and concentrated to adjust ph4, add Equal volume of ethyl acetate was extracted three times, the extract was washed three times with 5% sodium carbonate solution, and the ethyl acetate was recovered to obtain 7 g of crude product. Mix n-hexane, ethyl acetate, methanol, and water at a ratio of 5:5:3:4, and after standing for stratification, take the upper phase and fill the high-speed countercurrent chromatography column, turn the host, adjust the speed to 700rpm, and pump into the lower phase for flow Phase, after the dynamic equilibrium is established, the flow rate is adjusted to 2ml / min, and the crude product dissolved in the mobile phase is injected by the injection valve, and the ultraviolet detector ...

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Abstract

The invention belongs to the technical field of biology, and discloses a method for extracting 4-hydroxyderricin from angelica keiskei. The method is characterized in comprising the steps that: (1) angelica keiskei is crushed; 5-8 time amount of 30-60% ethanol is added, and ultrasonic extraction is carried out 2-3 timed; the extraction liquid is concentrated until no alcohol is left; polyamide resin column is added for absorption; 4-5BV 20-30% ethanol solution is used for eluting; an eluting liquid is concentrated, and a pH value is regulated to 3-5; ethyl acetate is added for extracting; an obtained extraction liquid is washed 3-4 timed by using a 5% sodium carbonate solution; and ethyl acetate is recovered, such that a crude product is obtained; and (2) n-hexane, ethyl acetate, methanol, and water are mixed; an upper-phase is used for filling a high-speed countercurrent chromatographic column; a main machine is rotated, and a lower-phase is pumped in as a mobile phase; the crude product dissolved by the mobile phase is fed by using a feeding valve, and is subjected to UV detector online monitoring; a target component is collected; obtained fractions are combined; and the mixture is subjected to reduced-pressure drying, such that high-purity 4-hydroxyderricin is obtained. The method provided by the invention has the advantages of high efficiency, large preparation amount, and high yield.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a method for extracting 4-hydroxydrysin from Ashitaba. Background technique [0002] 4-hydroxyderricin (4-hydroxyderricin) is a chalcone compound, CAS number 55912-03-3, molecular formula C 21 h 22 o 4 , the molecular structure is [0003] [0004] 4-Hydroxydrisin is a water-soluble yellow pigment with good antibacterial, anti-ulcer, anti-thrombotic, hypotensive, anti-allergic, anti-cancer, anti-AIDS, anti-dementia, anti-diabetes and many other effects. [0005] Ashitaba belongs to the Umbelliferae family and is native to Japan. It is also known as Duguancao, Longevity Grass, Juncao, Bazhangcao, Huanyangcao, God-given grass, etc. Ashitaba is rich in nutrients and comprehensive, known as the king of vegetables in Japan. Today, in Japan, South Korea, Taiwan and other places, Ashitaba has become an all-round food for "health, vitality and longevity". Modern research...

Claims

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Application Information

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IPC IPC(8): C07C49/255C07C45/79
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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