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Method for preparing arctin from burdock

A technology of arctiin and burdock fruit, which is applied in the field of preparing arctiin, can solve the problems that the silica gel column chromatography is not easy to scale up production, the one-time investment of equipment is large, and it is not suitable for industrialization, etc., and achieves long resin life and resin adsorption capacity Large, the effect of improving the adsorption capacity

Inactive Publication Date: 2010-06-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

"Extraction and Separation of Arctiin in Arctium Fructus" published by Lu Laichun, this document discloses a kind of alcohol extraction, macroporous adsorption resin and silica gel column chromatography separation and purification method, but silica gel column chromatography is not easy to amplify production; Dong Wenhong published "Experimental Research on the Extraction of Arctiin from Arctium Fructus by Supercritical Fluid", this document discloses the supercritical fluid extraction method, which has high extraction rate and less pollution, but the one-time investment of equipment is large, and it is not suitable for industrialization

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  • Method for preparing arctin from burdock

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Effect test

Embodiment 1

[0034] Get burdock fruit, pulverize, get 10kg, put into extraction tank, add 80L 75% ethanol, reflux extraction 1 hour, extract 2 times, combine 140L extract, add 800g activated carbon decolorization 2 hours. Filter the decolorized solution through a hollow fiber microfiltration membrane, and then pass the filtrate through a hollow composite ultrafiltration membrane with a molecular weight cut-off of 3000-6000 at a pressure of 0.8Mpa, collect the permeate, concentrate to an alcohol concentration of 20%, and add hydrochloric acid solution to adjust the pH to 4. Take 10LADS-17 macroporous adsorption resin and pack it into a column, treat and activate it, add the decolorization solution into the resin column at a flow rate of 15L / h, and wash it with 50L of water and 60L of 50% ethanol in turn, and detect it by thin-layer chromatography at the same time, and collect arctiin stream Minute, recover ethanol, concentrate to 15L, and grow crystals for 8 hours. Filter out 620 g of crud...

Embodiment 2

[0036] Take burdock fruit, crush it, take 10kg, put it into an extraction tank, add 60L of 90% ethanol, reflux extraction for 1 hour, extract 3 times, combine 160L of extracts, add 900g of activated carbon for 1 hour, and filter the decolorized solution through a hollow fiber microfiltration membrane. The filtrate passes through a hollow composite ultrafiltration membrane with a molecular weight cut-off of 6000-10000 at a pressure of 0.6Mpa, collects the permeate and concentrates it until the alcohol concentration is 25%, adjusts the pH to 3 by adding sulfuric acid solution, and adds 10LADS-17 at a flow rate of 10L / h The macroporous adsorption resin was eluted with 60L of water and 40L of 70% ethanol in turn, and detected by thin-layer chromatography at the same time, the fraction of arctiin was collected, the ethanol was recovered, concentrated to 12L, and the crystal was grown for 10 hours. Filter out 610 g of crude crystals, wash with petroleum ether, heat to dissolve with a...

Embodiment 3

[0038] Take burdock fruit, crush it, take 10kg, put it into an extraction tank, add 100L of 80% ethanol, reflux extraction for 1 hour, extract twice, combine 180L of extract, add 1000g of activated carbon for 2 hours, and filter the decolorized solution through a hollow fiber microfiltration membrane. The filtrate passes through a hollow composite ultrafiltration membrane with a molecular weight cut-off of 3000-6000 at a pressure of 0.8Mpa, collects the permeate, shrinks to an alcohol concentration of 30%, adds phosphoric acid solution to adjust the pH to 3, adds 10L of HZ806 macroporous adsorption resin, and uses 60L of water and 50L of 60% ethanol were eluted, and at the same time detected by thin-layer chromatography, the arctiin fraction was collected, the ethanol was recovered, concentrated to 10L, and grown for 15 hours. Filter out 320 g of crude crystals, wash with petroleum ether, heat dissolve in acetone, add dropwise 1% ether, grow crystals for 16 hours, crystallize t...

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Abstract

The invention relates to a method for preparing arctin from burdock, which adopts burdock medicinal material as the raw material and comprises the following steps: grinding the burdock medicinal material, reflux extracting for 2-3 times by ethanol, de-coloring by active carbon, concentrating to be low-concentration ethanol after microfiltration and ultrafiltration, adjusting pH, adsorbing by macro-porous absorption resin, eluting by water and ethanol, collecting burdock fraction, recovering a reagent, placing for crystallization, washing by petroleum ether and re-crystallizing by acetone and diethyl ether. The process is easy to enlarge production.

Description

Technical field: [0001] The invention relates to a method for preparing arctiin from burdock seeds, in particular to a method for preparing arctiin through microfiltration, ultrafiltration, separation and purification, and macroporous adsorption resin adsorption. Background technique: [0002] Arctiin is a lignanolide glycoside. [0003] Molecular formula: C 27 h 34 o 11 . [0004] Molecular weight: 534.55 [0005] The molecular structure is: [0006] [0007] nature: [0008] Arctiin is a colorless crystalline powder with a melting point of 110-112°C. [0009] Arctium has different degrees of inhibitory effects on a variety of pathogenic fungi. Arctiin has anti-pancreatic cancer activity, causing vasodilation, blood pressure drop, and convulsions in cold-blooded and warm-blooded animals. At the same time, it has anti-nephropathy effect, enhances the immune function of the body, has anti-complement activity, calcium antagonism, and antihypertensive pharmacology. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/26C07H1/08
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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