Preparation method for high-purity di-coffee mesitoyl quinine acid compounds

A caffeoylquinic acid, high-purity technology, applied in the separation/purification of carboxylic acid esters, medical preparations containing active ingredients, digestive systems, etc., can solve the problems of difficult separation and purification, high cost, low recovery rate, etc. , to achieve the effect of large separation capacity and strong performance

Inactive Publication Date: 2009-01-14
施树云 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Dicaffeoylquinic acid compounds are white powdery solids, easily soluble in hot water, hot methanol, hot ethanol, insoluble in ether, benzene and other less polar organic solvents, and oxidatively decomposed or transformed into other dicaffeoylquinic acid compounds when heated. Acylquinic acid compounds, in addition, the three compounds are unstable in solution and can be transformed into each other, which causes great difficulties for their separation and purification
These methods are complicated in steps, time-consuming and laborious, and the recovery rate is low, the cost is high, and they are not suitable for industrialization.

Method used

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  • Preparation method for high-purity di-coffee mesitoyl quinine acid compounds
  • Preparation method for high-purity di-coffee mesitoyl quinine acid compounds
  • Preparation method for high-purity di-coffee mesitoyl quinine acid compounds

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Embodiment Construction

[0027]1. Dried the whole herb of Mongolian dandelion at 50°C and pulverized. Take 200g of crude drug, put it in a 2000mL round bottom flask, add 1600mL of 75% ethanol, reflux extraction 3 times, each time for 2h, filter, combine the filtrates, concentrate under reduced pressure until no alcohol smell, and recover the organic solvent. The concentrated solution is subjected to D101 macroporous adsorption resin column chromatography, washed with water until it has no alcohol smell, and then eluted with 20% and 40% ethanol aqueous solution in sequence, and the 40% ethanol eluate is collected and concentrated under reduced pressure until it is alcohol-free smell, add ethanol until the alcohol content is 80%, filter off the precipitate, take the supernatant and vacuum-dry to obtain the crude product of dicaffeoylquinic acid compounds. The crude product was separated and purified by high-speed countercurrent chromatography under the following conditions: rotation speed: 800rpm; solve...

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Abstract

The invention discloses a method for preparing a high purity dicaffeoylquinic acid compound by high-efficient separation, mainly comprising: using an alcohol-water solution to extract taraxacum fresh plant or dry plant, carrying out the column chromatographic separation after the concentration, preparing a crude extract rich in dicaffeoylquinic acid compound, then isolating and purifying the crude extract by high-speed countercurrent chromatography, and finally adopting a recrystallization process for refining so as to obtain 3,5-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid with high purity. The method is applied to the preparation of high purity monomers by taking various natural products or natural product extracts containing one or a plurality of ingredients in the dicaffeoylquinic acid compound and acquired through various approaches as raw materials, and has advantages of simple steps, simple operation, high efficiency, low cost, easy repetition, and large output of separation and preparation. The purity of dicaffeoylquinic acid compound prepared by the method can reach 98 percent.

Description

technical field [0001] The present invention relates to a method for separating and purifying active ingredients in traditional Chinese medicine or natural products, mainly to a method for extracting and separating monomeric compounds from traditional Chinese medicine or natural products, in particular to a high-purity 3,5-dicaffeoylquinic acid, 3 , The separation and preparation method of 4-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid. Background technique [0002] Dandelion is a well-known Chinese herbal medicine and wild vegetable in my country. It is the dried whole herb of Taraxacum mongolicum Hand.-Mazz., Taraxacum sinicum Kitag. or several plants of the same genus. It is widely distributed in Northeast China. , North China, Northwest, Central China, East China and Southwest provinces and autonomous regions, with the most in Southwest and Northwest China. Have heat-clearing and toxic substances removing, reducing swelling and dissipating stagnation, inducing diu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/48A61P37/00A61P31/12A61P1/16A61P31/18A61P39/06A61K36/288
Inventor 施树云张宇平
Owner 施树云
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