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Alkynyl glycoside compound and extraction and separation method and application thereof

A separation method and compound technology, which are applied in chemical instruments and methods, medical preparations containing active ingredients, sugar derivatives, etc., can solve the problems of large solvent consumption, low content, and cumbersome solvent recovery, and achieve the effect of rapid purification.

Active Publication Date: 2017-07-11
INST OF SPECIAL ANIMAL & PLANT SCI OF CAAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The types of existing alkyne glycosides are limited and the content is very low; and the existing extraction methods are time-consuming, consume a lot of solvents, and the recovery of solvents is cumbersome

Method used

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  • Alkynyl glycoside compound and extraction and separation method and application thereof
  • Alkynyl glycoside compound and extraction and separation method and application thereof
  • Alkynyl glycoside compound and extraction and separation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Take platycodon root powder that has passed through a 200-mesh sieve, and ultrasonically extract it with 10, 8, and 6 times the amount of methanol in sequence. The first extract: dissolve the first extract with distilled water, and the solution obtained is adsorbed with AB-8 weakly polar macroporous resin, and the first time is carried out with water of 8 times column volume and 30% ethanol by volume fraction Part of the sugar and inorganic salts and other substances in the solution are eluted to remove, and then the ethanol with a volume fraction of 50% is used for the second elution to enrich the polyacetylene components, and the eluate after the second elution is concentrated for the second time , to obtain the second extract; use countercurrent chromatography with n-hexane: ethyl acetate: methanol: water (1:31:1:31, v / v / v / v) as the solvent system, flow rate 5mL / min, speed 800r / s, separate and purify the second extract, and take the effluent of polyalkyne components...

Embodiment 2

[0055] Take platycodon root powder that has passed through a 300-mesh sieve, and ultrasonically extract it with 9 and 7 times the amount of methanol in sequence. Extract: dissolve the first extract with distilled water, absorb the obtained solution with AB-8 weakly polar macroporous resin, and first elute with 40% ethanol to remove part of the sugar and Inorganic salts and other substances, and then use ethanol with a volume fraction of 60% to carry out the second elution to enrich the polyacetylene components, and the eluent after the second elution is concentrated for the second time to obtain the second extract; Chromatography uses n-hexane: ethyl acetate: methanol: water (1:28:1:32, v / v / v / v) as the solvent system, the flow rate is 4mL / min, the rotation speed is 800r / s, and the second extract is separated and purified. And according to the countercurrent chromatogram, take the effluent of the polyalkyne component; after the polyalkyne component effluent is concentrated unde...

Embodiment 3

[0057] The platycodon root powder passed through a 250-mesh sieve was ultrasonically extracted with 10 and 8 times the amount of methanol in sequence, and the time of each extraction was 0.3h. The extracted liquid was filtered and combined to obtain the extract, which was concentrated under reduced pressure to obtain the first Extract: dissolve the first extract with distilled water, absorb the obtained solution with AB-8 weakly polar macroporous resin, and first elute with 20% ethanol to remove part of the sugar and Substances such as inorganic salts, and then use ethanol with a volume fraction of 55% to carry out the second elution to enrich the polyacetylene components, and the eluent after the second elution is concentrated for the second time to obtain the second extract; Chromatography uses n-hexane: ethyl acetate: methanol: water (1:32:1:28, v / v / v / v) as the solvent system, the flow rate is 6mL / min, the rotation speed is 800r / s, and the second extract is separated and pur...

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Abstract

The invention relates to an alkynyl glycoside compound and an extraction and separation method and an application thereof, and belongs to the field of extraction and separation of natural compounds. The extraction and separation method comprises the steps: carrying out ultrasonic extraction of a patycodon grandiflorum powder, and concentrating the extract liquid to obtain a first extractum; adding water to the first extractum, dissolving, then adding to adsorption resin, carrying out gradient elution with ethanol, and concentrating the eluate of gradient elution for a second time to obtain a second extractum; carrying out countercurrent chromatography separation and purification of the second extractum with a solvent system of n-hexane, ethyl acetate, methanol and water with a volume ratio of 1:(28-32):1:(28-32), and collecting polyacetylene compound effluent; and concentrating the polyacetylene compound effluent for a third time, and preparing with a high performance liquid chromatograph and with acetonitrile-water as a mobile phase. The method is efficient and fast; and the purified alkynyl glycoside compound has antimicrobial and antitumor activities and the like, and can be applied to preparation of anti-biological toxicity drugs.

Description

technical field [0001] The invention relates to the field of extraction and separation of natural compounds, and in particular to alkyne glycoside compounds and their extraction and separation methods and applications. Background technique [0002] Polyacetylene is a relatively special natural compound, which is mainly distributed in plant tissues such as Compositae, Platycodonaceae, Araliaceae, Umbelliferae and Pittogoniaceae. Its antimicrobial, cytotoxic and antitumor activities etc. have good biological activity. The types of the existing alkyne glycosides are limited, and the content is very low; and the existing extraction method is time-consuming, consumes a large amount of solvent, and the recovery of the solvent is cumbersome. Contents of the invention [0003] The object of the present invention is to provide an alkyne glycoside compound, which has good biological activity in terms of antimicrobial, cytotoxic and antitumor activities, and can be applied to the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/10C07H1/08A61K31/7032A61P31/00A61P39/02A61P35/00
CPCC07H1/08C07H15/10
Inventor 刘政波陈宝芳
Owner INST OF SPECIAL ANIMAL & PLANT SCI OF CAAS
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