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Method for preparing high-purity aucubin

A high-purity technology of aucubin, applied in the field of medicine, can solve the problems of high price of high performance liquid chromatography, can only reach milligram level, limited amount of preparation, etc. Effect

Inactive Publication Date: 2010-10-20
NANJING ZELANG AGRI DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] At present, there are few researches on the extraction process of aucubin. Chinese patent 200810017377.2 discloses "a method for extracting aucubin from Artemisia spp. Crystallization, this method takes a long time to extract, the yield is low, a large amount of methanol solution is used, the toxicity is high, and there are certain potential safety hazards
Chinese patent 200810031122.1 discloses "a method for extracting iridoid active parts and monomers from Eucommia ulmoides", this method requires high-performance liquid chromatography and requires expensive instruments, and the amount of preparation is limited, generally only up to Milligram Separation

Method used

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  • Method for preparing high-purity aucubin

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Effect test

Embodiment 1

[0036] Pulverize Eucommia leaves to 40 mesh, put 20kg into the extraction tank, add 160L n-hexane to degrease, degrease twice, each time for 2 hours, filter out the dregs as degreasing crude material. 120 L of 50% ethanol solution was added to the degreased crude material for ultrasonic extraction for 30 minutes, and the extracts were extracted three times, and the extracts were combined. Take 20LHPD100 macroporous adsorption resin to pack into a column, pretreat, add the extract to the resin column, and sequentially elute with 5BV of water, 4BV of 10% ethanol, 4BV of 20% ethanol, and 5BV of 30% ethanol. Glycoside fraction, recovered ethanol, concentrated to no alcohol smell, pumped the concentrated solution into a 10L medium-pressure silica gel column, first pumped 8BV of water and then pumped 5BV of 10% ethanol to elute, TLC detection, collected aucubin fraction, Concentrate under reduced pressure at 50°C to 1 / 8 of the original volume, add acetone to saturate and dissolve, a...

Embodiment 2

[0038] Grind Artemisia chinensis to 20 mesh, take 20kg and put it into an extraction tank, add 200L n-hexane to degrease, degrease 3 times, each time for 1.5 hours, filter out the dregs as degreasing coarse material. Add 100L of 60% ethanol solution to the degreased crude material for ultrasonic extraction for 45 minutes, extract twice, and combine the extracts. Take 20LAB-8 macroporous adsorption resin and put it into a column, pretreat it, add the extract to the resin column, wash it with 6BV of water, 4BV of 10% ethanol, 3BV of 20% ethanol, and 5BV of 30% ethanol. For the fraction of phyllobornins, recover ethanol, concentrate until there is no alcohol smell, pump the concentrated solution into a 10L medium-pressure silica gel column, first pump 5BV of water and then pump 6BV of 10% ethanol for elution, TLC detection, and collect aucubin stream Minute, concentrate under reduced pressure at 50°C to 1 / 10 of the original volume, add acetone to saturate and dissolve, add a smal...

Embodiment 3

[0040] Crush the eucommia seed kernels to 50 mesh, put 10kg into the extraction tank, add 90L n-hexane to degrease, degrease twice, each time for 1.5 hours, and filter out the dregs as degreasing crude material. Add 80L of 40% ethanol solution to the degreased crude material for ultrasonic extraction for 1 hour, extract twice, and combine the extracts. Take 10LHPD-600 macroporous adsorption resin to pack into a column, pretreat, add the extract to the resin column, and sequentially elute with 5BV of water, 6BV of 10% ethanol, 4BV of 20% ethanol, and 4BV of 30% ethanol. For the fraction of phyllobornin, recover ethanol, concentrate until it has no alcohol smell, pump the concentrated solution into a 10L medium-pressure silica gel column, first pump 6BV of water and then pump 5BV of 10% ethanol for elution, TLC detection, and collect aucubin stream Minute, concentrate under reduced pressure at 40°C to 1 / 9 of the original volume, add acetone to saturate and dissolve, add a small ...

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Abstract

The invention belongs to the technical field of medicines and relates to a method for preparing high-purity aucubin. In the method, normal hexane is degreased, and the residues are soaked in water or aqueous solution of ethanol for ultrasonic extraction; the obtained extract is passed through a chromatographic column of a polymer filler solid phase, the chromatographic column is eluted by a small amount of water and low-concentration aqueous solution of ethanol, the separated product is concentrated, the concentrate is separated by a silicagel column and recrystallization is performed to obtain the high-purity aucubin. The method has the advantages that: products can be produced in large scale and with high purity; the adopted polymer filler solid phase and the adopted silicagel column can be used repeatedly; the cost is low; the organic phase used for elution is free from organic solvents which have high toxicity and cause heavy pollution to environment; and the recovered organic phase can be used repeatedly.

Description

Technical field: [0001] The invention belongs to the technical field of medicine and relates to a method for preparing high-purity aucubin. Background technique: [0002] Aucubin is an iridoid glycoside. [0003] Molecular formula: C 15 h 22 o 9 ; [0004] Molecular weight: 346.33; [0005] Molecular formula: [0006] [0007] Physical and chemical properties: Melting point 181°C (ethanol-ether), easily soluble in water, methanol, soluble in ethanol, insoluble in ether, chloroform, benzene and petroleum ether. [0008] Aucubin (AU) is widely found in plants, especially Eucommia ulmoides, Psyllium chinensis, Rehmannia glutinosa, Artemisia genus and Aucubinia genus. Pharmacological studies have shown that AU has the functions of protecting the liver and detoxification, anti-inflammation, anti-oxidation, anti-aging, anti-osteoporosis, and neurotrophy, and is widely used in the health care industry. [0009] At present, there are few researches on the extraction proce...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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