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Method for rapidly and efficiently preparing aucubin monomer from eucommia ulmoides

An aucubin, fast technology, applied in the field of medicine, can solve the problems of cumbersome operation, large consumption of reagents, high cost, etc., and achieve the effect of broad development prospects, simple environmental protection process, and low equipment requirements

Inactive Publication Date: 2013-06-26
JISHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it has been reported to extract aucubin from Eucommia ulmoides (Li Qin, Du Hongyan, Zhang Musheng, etc. A method for extracting aucubin from Eucommia ulmoides seed meal, patent application number 201110136082.9; Liu Yuming, Chen Baoquan, Li Caiwen, etc. A A process for extracting aucubin from eucommia fruit, patent application number 201010297478.7; Zhang Kangjian. A method for continuously extracting eucommia oil and aucubin from eucommia seeds, patent application number 01128744.6), but they all use extraction Or macroporous adsorption resin method and other separation and purification methods, the obtained aucubin product has low purity, large reagent consumption, cumbersome operation, long industrial production cycle, and high cost

Method used

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  • Method for rapidly and efficiently preparing aucubin monomer from eucommia ulmoides
  • Method for rapidly and efficiently preparing aucubin monomer from eucommia ulmoides
  • Method for rapidly and efficiently preparing aucubin monomer from eucommia ulmoides

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take 1 kg of Eucommia ulmoides leaf powder of 40 mesh and place it in a flat-bottomed flask, add 5 L of methanol or ethanol / ethyl acetate = 1:1 (volume ratio) mixed solvent, carry out ultrasonic reflux extraction at 60 ° C for 0.5 h, and recover the solvent to a certain volume , cooled, the obtained light brown precipitate was dissolved by adding methanol or ethanol at a ratio of 1:8 to solid-liquid, and then adding ethyl acetate or chloroform according to 3 times the volume of methanol or ethanol, condensing and refluxing for 0.5h, filtering while hot, and keeping the filtrate from light at room temperature After standing for 10 hours, white granular crystals were precipitated, which were naturally volatilized and dried to obtain 30 g of aucubin monomer. The content of aucubin monomer was determined by HPLC method to reach 81%, and the above crystallization treatment was repeated, and the content could reach more than 95%.

Embodiment 2

[0024] Take 1 kg of eucommia bark powder of 40 mesh and place it in a flat-bottomed flask, add 10 L of methanol or ethanol / ethyl acetate = 1:8 (volume ratio) mixed solvent, conduct ultrasonic reflux extraction at 75 °C for 1 hour, repeat the extraction once, and combine Filtrate, recover the solvent to a certain volume, cool, add methanol or ethanol to dissolve the obtained light brown precipitate at a solid-liquid ratio of 1:12, add ethyl acetate or chloroform according to 4.5 times the volume of methanol or ethanol, condense and reflux for extraction for 1 h, and After hot filtration, the filtrate was kept at room temperature and protected from light for 24 hours, white granular crystals were precipitated, and dried at low temperature to obtain 35 g of aucubin monomer. Repeat the above crystallization treatment, and the content can reach more than 95%.

Embodiment 3

[0026] Take 1 kg of eucommia ulmoides seed meal powder of 60 mesh and put it in a flat-bottomed flask, add 15 L of methanol or ethanol / ethyl acetate = 1:15 (volume ratio) mixed solvent, conduct ultrasonic reflux extraction at 75 ° C for 1.5 h, and repeat the extraction twice , combine the filtrates, recover the solvent to a certain volume, cool, and add methanol or ethanol to heat and dissolve the obtained light brown precipitate at a solid-liquid ratio of 1:15, then add ethyl acetate or chloroform according to 6 times the volume of methanol or ethanol, and condense and reflux for extraction for 2 hours , filtered while it was hot, and the filtrate was kept at room temperature in the dark for 48 hours, white granular crystals were precipitated, dried with nitrogen, and 39 g of aucubin monomer was obtained, and its content was 95% as determined by HPLC.

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Abstract

The invention provides a method for rapidly and efficiently preparing an aucubin monomer from eucommia ulmoides. The method disclosed by the invention comprises the following steps of: taking eucommia ulmoides leaves / peels / seed cakes as raw materials; adding methanol or ethyl acetate according to a certain ratio to carry out ultrasonic reflowing and extraction; filtering; decompressing a filtering solution and recycling a solvent to a suitable amount; after cooling, separating light brown sediment; adding suitable amounts of ethyl acetate-methanol; condensing and reflowing; hotly filtering; standing at a room temperature; and separating sediments and filtering to obtain a white grain crystal of aucubin. The method disclosed by the invention adopts abundant raw material resources and the aucubin monomer can be prepared by two steps of extracting and crystallizing; and the method has an environment-friendly and simple process, is low in equipment requirements and can easily realize industrialized production. The industrial production of the aucubin enhances development and utilization values of the eucommia ulmoides in fields of medical treatment and health care, and brings about economic and social benefits.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for rapidly and efficiently preparing aucubin monomer from Eucommia ulmoides. Background technique [0002] Aucubin (AU) is an iridoid compound with the molecular formula C 15 h 22 o 9 . The molecular weight is 346.33. It is white needle-like crystal in ethanol. The melting point is 181°C. It is easily soluble in polar solvents such as water, methanol and ethanol, and almost insoluble in weak polar solvents such as petroleum ether, chloroform and ether. The molecule of aucubin contains hemiacetal structure, which is active and easy to decompose when encountering acid, alkali, heat, light, oxygen, etc. Scholars at home and abroad have found that aucubin and its derivatives have liver protection and detoxification, anti-inflammatory, anti-oxidation, anti-aging, anti-osteoporosis and other effects. [0003] Eucommia ( Eucommia ulmoides Oliv) is a perennia...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 彭密军彭胜郭婕张琳杰张昌伟王志宏
Owner JISHOU UNIVERSITY
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