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Method for simultaneous preparation of rhamnocitrin and rhamnazin chemical reference substances

A technology of rhamnetin and rhamnetin, which is applied in the direction of organic chemistry, etc., can solve the problems of no rhamnetin and rhamnetin reference substance supply, and no rhamnetin and rhamnetin chemical reference substances, etc. The effect of low separation cost and simple process

Inactive Publication Date: 2015-04-22
四川医科大学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, there is no chemical reference substance of rhamnolimonin and rhamnosin in the country, and there is no supply of rhamnocitrin and rhamnosin reference substance on the market.

Method used

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  • Method for simultaneous preparation of rhamnocitrin and rhamnazin chemical reference substances
  • Method for simultaneous preparation of rhamnocitrin and rhamnazin chemical reference substances
  • Method for simultaneous preparation of rhamnocitrin and rhamnazin chemical reference substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Petroleum ether degreasing: crush 10 kg of blue skyflower into a coarse powder, heat and reflux 7 times with 6 times the amount of petroleum ether at 60-90° C., 1 hour each time. Filter, and evaporate the residue of the blue skyflower to dryness with petroleum ether.

[0027] (2) Ethyl acetate extraction: Add 5 times the amount of ethyl acetate to the degreased N. cerevisiae residue and heat to reflux for 6 times, 1 hour each time. The ethyl acetate extracts were combined, the solvent was recovered, and dried under vacuum at 60°C for 24 hours to obtain 96.1 g of extract.

[0028] (3) Silica gel column chromatographic separation: the dried ethyl acetate part extract was separated by silica gel column chromatography. Take 60g of the ethyl acetate extract and dissolve it in 2 times of absolute ethanol, mix it with 100-200 mesh column chromatography silica gel at a ratio of 1:2, and dry it in vacuum at a constant temperature of 50°C for 12 hours. Take 900g of fresh sil...

Embodiment 2

[0031] (1) Petroleum ether degreasing: crush 10 kg of blue skyflower into a coarse powder, heat and reflux 6 times with 8 times the amount of petroleum ether at 60-90° C., 1 hour each time. Filter, and evaporate the residue of the blue skyflower to dryness with petroleum ether.

[0032] (2) Ethyl acetate extraction: Add 6 times the amount of ethyl acetate to the degreased N. cerevisiae residue and heat to reflux for 6 times, 1 hour each time. The ethyl acetate extracts were combined, the solvent was recovered, and dried under vacuum at 60°C for 24 hours to obtain 100 g of extract.

[0033] (3) Silica gel column chromatographic separation: the dried ethyl acetate part extract was separated by silica gel column chromatography. Take 60g of the ethyl acetate extract and dissolve it in 2 times of absolute ethanol, mix it with 200-300 mesh column chromatography silica gel at a ratio of 1:2, and dry it in vacuum at a constant temperature of 50°C for 12 hours. Take 900g of fresh sili...

Embodiment 3

[0036] (1) Petroleum ether degreasing: crush 10 kg of blue skyflower into a coarse powder, heat and reflux 8 times with 6 times the amount of petroleum ether at 60-90° C., 1 hour each time. Filtration, and evaporate the residue of the blue skyflower to dry petroleum ether.

[0037] (2) Ethyl acetate extraction: Add 7 times the amount of ethyl acetate to the degreased N. radix residue and heat to reflux for 6 times, 1 hour each time. The ethyl acetate extracts were combined, the solvent was recovered, and dried under vacuum at 60°C for 24 hours to obtain 98.1 g of extract.

[0038] (3) Chromatographic separation of polyamide: the dried ethyl acetate extract was separated by polyamide column chromatography. Take 60g of the ethyl acetate extract and dissolve it in 2 times absolute ethanol, mix it with 100-200 mesh polyamide at a ratio of 1:1.5, and dry it in vacuum at a constant temperature of 50°C for 12 hours. Take 1500g of pretreated polyamide and pack it into a column , fol...

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Abstract

A stiff paste-like ethyl acetate extract is obtained by extracting nervilia fordii with petroleum ether through heating reflux, extracting residues with ethyl acetate through heating reflux, and recovering ethyl acetate. The ethyl acetate extract is separated by silica gel column chromatography or polyamide chromatography; components of rhamnocitrin and rhamnazin are collected and combined by silica gel thin layer chromatography or a hydrochloric acid-magnesium powder chemical identification method; after solvent recovery, a crude product (yellow powder) of a mixture of rhamnocitrin and rhamnazin is obtained; the crude product is separated by reversed-phase high performance liquid chromatography to obtain two chemical reference substances of rhamnocitrin and rhamnazin with purity of more than 98%. The method of the invention is simple in process step, high in purity, good in product color, and large in preparation capacity.

Description

1. Technical field [0001] The invention relates to a method for simultaneously preparing two chemical reference substances, rhamnolimonin and rhamnosin, from the traditional Chinese medicine Qingtiankui. It belongs to the field of traditional Chinese medicine modernization. It mainly includes four steps: degreasing petroleum ether, extracting ethyl acetate, separating by silica gel column chromatography or polyamide column chromatography, and refining by reversed-phase high-performance liquid chromatography to obtain two chemical compounds, rhamnolimonin and rhamnatin. Control substance. The structures of the two reference substances are as follows: [0002] 2. Background technology [0003] Qingtiankui is derived from the underground tubers and whole plants of NerviliaFordii (Hance) Schltr, a plant of the Orchidaceae family. It is mainly distributed in Guangdong, Guangxi, Sichuan, Yunnan, Guizhou and other provinces and regions. It is a traditional Chinese medicine in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/40C07D311/30
CPCC07D311/30C07D311/40
Inventor 袁叶飞
Owner 四川医科大学
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