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Preparation method for mussaendoside U

A technology of Jade leaf golden flower and ethanol solution, which is applied in the field of natural medicinal chemistry, can solve the problems of low product purity and low yield, and achieve the effects of high purity, convenient operation, and simple and reasonable process

Inactive Publication Date: 2014-04-23
GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing method for separating mussaendoside U generally adopts reversed-phase silica gel column chromatography and Sephadex column chromatography, and the resulting product has a purity lower than 90% and a lower yield

Method used

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  • Preparation method for mussaendoside U

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The raw material powder is 5kg Yuyejinhua coarse powder mixed with 60% ethanol with a volume concentration 8 times the weight of the raw material powder, heated and refluxed for extraction 3 times, each time for 2 hours, the extract is concentrated in vacuum to recover the solvent to obtain a crude extract extract. The obtained extract was miscible with water, and then an equivalent amount of water-saturated n-butanol was added to extract for 3 times. The organic layers were combined and concentrated in vacuo to obtain an extract-like substance, which was dissolved in water and filtered, and the filtrate was applied to a D101 macroporous resin chromatography column. Use distilled water, 20% ethanol, 40% ethanol, 60% ethanol, 95% ethanol solution to elute sequentially, collect 60%-95% ethanol eluate, recover ethanol, evaporate to dryness until the water content is 15%, that is, total saponins Crude product; the total saponin crude product was dissolved in methanol, and se...

Embodiment 2

[0021] The raw material powder is 5kg Yuyejinhua coarse powder mixed with 95% ethanol with a volume concentration 10 times the weight of the raw material powder, heated and refluxed for 3 times, each time for 2 hours, the extract is concentrated in vacuum to recover the solvent to obtain a crude extract. The obtained extract was miscible with water, and then an equivalent amount of water-saturated n-butanol was added to extract for 3 times. The organic layers were combined and concentrated in vacuo to obtain an extract-like substance, which was dissolved in water and filtered, and the filtrate was applied to a D101 macroporous resin chromatography column. Use distilled water, 20% ethanol, 40% ethanol, 60% ethanol, 95% ethanol solution to elute sequentially, collect 60%-95% ethanol eluate, recover ethanol, evaporate to dryness until the water content is 14%, that is, the crude product of total saponins ; The total saponin crude product was dissolved in methanol and separated by ...

Embodiment 3

[0023] Mix 5 kg of raw material powder Yuye Jinhua coarse powder with 95% ethanol which is 8 times the weight of the raw material powder, heat and reflux extraction for 3 times, each time for 2 hours, vacuum concentrate the extract to recover the solvent to obtain a crude extract extract. The obtained extract was miscible with water, and then an equal amount of water-saturated n-butanol was added to extract for 3 times. The organic layers were combined and concentrated in vacuo to obtain an extract-like substance, which was dissolved in water and filtered, and the filtrate was applied to a DA201 macroporous resin chromatography column. Use distilled water, 20% ethanol, 40% ethanol, 60% ethanol, and 95% ethanol solution to elute sequentially, collect 60%-95% ethanol eluate, recover ethanol, evaporate to dryness until the water content is 13%, and obtain total saponins Crude product; the total saponin crude product was dissolved in methanol and separated by HPLC preparative chrom...

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Abstract

A disclosed preparation method for mussaendoside U comprises the following steps: (1) adding mussaenda pubescens coarse powder into an ethanol solution, heating, refluxing and extracting, recovering ethanol and obtain a crude extract product; (2) adding distilled water into the crude extract product, mixing and dissolving, then adding water-saturated n-butanol and extracting for multiple times, concentrating to obtain an extractum-like substance; (3) adding distilled water into the above extractum, dissolving and filtering, performing primary purification on the filtrate by macroporous resin column chromatography, and performing separation by HPLC preparative chromatography to obtain high-purity mussaendoside U. The method provided by the invention is simple and reasonable, operation is convenient, yield is high, purity is high, and mussaendoside U can be prepared into a standard substance.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a preparation method of mussaendoside U. Background technique [0002] mussaendoside U is a tetracyclic triterpene saponin with a molecular formula of C72H115NO32 and a molecular weight of 1505. The molecular structure is: [0003] [0004] mussaendoside U is the main component of Rubiaceae plant Yuyejinhua. Jade leaf golden flower has the effect of clearing heat and relieving summer heat, cooling blood and detoxifying. Jade leaf golden flower is rich in terpenoids and triterpenoid saponins. At present, Yuye Jinhua has been widely used in Chinese patent medicines. The first Chinese patent medicine for treating influenza A in my country - Jinhua Qinggan Fang contains Yuye Jinhua; at the same time, Yuye Jinhua is used as a monarch drug in Yuye Jiedu Granules and Yuye Qinghuo Tablets use. [0005] The existing method for separating mussaendoside U general...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J53/00
Inventor 李嘉张颖张赟赟杨海船陈锋何春欢姜平川李红
Owner GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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